Tag: M.W=0-100

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 15518-10-2, name is 3-Amino-2-methylpropan-1-ol, molecular formula is C4H11NO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. name: 3-Amino-2-methylpropan-1-ol

EXAMPLE I N-(2-Hydroxy-1,1-dimethylethyl)-2,4,5-trifluorobenzamide A solution of 19.4 g (110 mmol) of 2,4,5-trifluorobenzoic acid (JP 58,150,543 (Cl. C07C69) Sept. 7, 1983). 15.2 g (120 mmol) of oxalyl chloride and 250 ml of dichloromethane was treated with four drops of DMF, and the mixture was stirred at room temperature for four hours. The mixture was concentrated to a oil and was redissolved in 100 ml of dichloromethane. This solution was added dropwise to a solution of 19.6 g (240 mmol) of 3-amino-2-methyl-1-propanol in 200 ml of dichloromethane at 5 C., and the reaction mixture was stirred at room temperature overnight. The solids were filtered, and the filtrate was washed with 5% sodium bicarbonate, 1N hydrochloric acid, and water. The organic layer was dried over magnesium sulfate and concentrated to give 24.5 g of the title compound, mp 114-116 C.

With the rapid development of chemical substances, we look forward to future research findings about 15518-10-2.

Reference:
Patent; Warner-Lambert Company; US4920120; (1990); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.33420-52-9, name is 2,2-Difluoropropan-1-ol, molecular formula is C3H6F2O, molecular weight is 96.076, as common compound, the synthetic route is as follows.Product Details of 33420-52-9

Trifluoromethanesulfonic anhydride (9.34 mL, 55.2 mmol) was added to a solution of 2,2-difluoropropan-1-ol (5.05 g, 52.6 mmol) in DCM (100 mL) at -10 C followed by dropwiseaddition of 2,6-dimethylpyridine (7.35 mL, 63.1 mmol) in DCM (50 mL). The reaction was stirred for 1 hour before addition of 2N HC1 (150 mL). The layers were separated and the aqueous phase was extracted with DCM (100 mL), then the combined organics were dried and concentrated carefully (no lower than 200 mbar, 40 C) to afford 2,2-difluoropropyltrifluoromethanesulfonate (12.90 g) as a brownlred oil that was used directly in next stage.2,2-Difluoropropyl trifluoromethanesulfonate (11.91 g, 52.22 mmol) was added to a solution of (R)-1-(1H-indol-3-yl)propan-2-amine (6.50 g, 37.3 mmol) and DIPEA (12.9 ml, 74.6 mmol) in 1 ,4-dioxane (75 mL) and the reaction was then heated to 65 C for 1.5 hours. The reaction was cooled to room temperature and diluted with EtOAc (250 mL). This waswashed with water (2 x 100 mL) and saturated aqueous sodium chloride (100 mL). The organic phase was separated and dried (MgSO4), filtered and evaporated. The crude product was purified by flash silica chromatography, elution gradient 0 to 10% MeOH in DCM to afford (R)-N-( 1 -(1 H-indol-3 -yl)propan-2-yl)-2,2-difluoropropan- 1-amine (7.99 g, 85%) as an orange/brown oil. ?H NMR (500 MHz, CDC13, 27 C) 1.11 (3H, d), 1.58 (3H, t), 2.77 -3.00 (4H, m), 3.07 (1H, h), 7.04 (1H, d), 7.12 (1H, ddd), 7.19 (1H, ddd), 7.36 (1H, dt), 7.57- 7.62 (1H, m), 8.03 (1H, s). (One proton not observed). m/z: ES+ [M+H]+ 253.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,33420-52-9, 2,2-Difluoropropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; ASTRAZENECA AB; SCOTT, James, Stewart; MOSS, Thomas, Andrew; YANG, Bin; VARNES, Jeffrey, Gilbert; O’DONOVAN, Daniel, Hillebrand; NISSINK, Johannes, Wilhelmus, Maria; HUGHES, Samantha, Jayne; BARLAAM, Bernard, Christophe; WU, Dedong; BROO, Dan, Anders; (224 pag.)WO2018/19793; (2018); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 2919-23-5, Cyclobutanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Formula: C4H8O, blongs to alcohols-buliding-blocks compound. Formula: C4H8O

A quartz glass tube charged with 50 g of catalyst (H1044, composition approx. 27 g of copper oxide, approx. 4 g of chromium oxide, approx. 5 g of barium oxide, on SiO2) and bounded at both ends with Raschig rings was installed in a commercial, electrically heated laboratory tubular furnace and the temperature in the catalyst zone was set to 200 C. 30 g of crude cyclobutanol product (purity approx. 73%, 0.3 mol) were evaporated using a preevaporator and then passed over the catalyst (LHSV=0.18/h). After leaving the catalyst zone, the reaction mixture was cooled using a condenser and collected in a cold trap. 27 g of reaction effluent were obtained, having a composition of 59% of cyclobutanone and 19% of cyclobutanol (conversion: 77%, selectivity: 96%). Example 7 Gas Phase Dehydrogenation [0043] In the experimental apparatus described in Example 6 (same catalyst), 256 g of crude cyclobutanol (purity approx. 74%) were converted at 250 C. (LHSV=0.33/h). 243 g of reaction effluent were obtained having an average composition of 63% of cyclobutanone and 12% of cyclobutanol (conversion: 84%, selectivity >98%). Distillation of the product mixture through a 1 m Multifil column provided 102 g of cyclobutanone in a purity of >99% (b.p.: 97-99 C., distillation yield: 67%). Example 8 Gas Phase Dehydrogenation [0044] The quartz glass tube was filled with 50 g of catalyst (H1044, calcined at 700 C.) and was stored in the laboratory tubular furnace as in Example 7. Likewise as described, 135 g (1.3 mol) of crude cyclobutanol (purity 71%) were passed over the catalyst at 250 C. (LHSV=0.33/h). 127 g of reaction effluent were obtained having an average composition of 58% of cyclobutanone and 2.5% of cyclobutanol (conversion: 97%, selectivity: 82%). Example 9 Gas Phase Dehydrogenation [0045] The quartz glass tube was filled with 50 g of catalyst (H1044, calcined at 650 C.) and stored in the laboratory tubular furnace as described in Example 7. 776 g of crude cyclobutanol (purity: 71%) were then passed in gaseous form over the catalyst at 250 C. (LHSV=0.33/h). 719 g of reaction effluent were obtained having an average composition of 67% of cyclobutanone and 5% of cyclobutanol (conversion: 94%, selectivity: 97%). Distillation of the product mixture through a 1 m Multifil column resulted in 380 g of cyclobutanone (purity >95%, distillation yield 81%). Example 10 Gas Phase Dehydrogenation [0046] The quartz glass tube was filled with 50 g of catalyst (H1044, calcined at 650 C.) and stored in the laboratory tubular furnace as described in Example 7. 876 g of crude cyclobutanol (purity: 75%) were then passed in gaseous form over the catalyst at 250 C. (LHSV=1.5 h-1). 832 g of reaction effluent were obtained having an average composition of 67% of cyclobutanone and 8% of cyclobutanol (conversion: 90%, selectivity: 97%). Distillation of the product mixture through a 1 m Multifil column resulted in 516 g of cyclobutanone (purity >95%, distillation yield 80%)

The synthetic route of 2919-23-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Degussa AG; US2004/254401; (2004); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 124-68-5, 2-Amino-2-methyl-1-propanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, 124-68-5, blongs to alcohols-buliding-blocks compound. name: 2-Amino-2-methyl-1-propanol

(1) Acetic acid (5.4 ml) was added to a solution of 2-amino-2-methyl-1-propanol (8.4 g) and benzaldehyde (10 g) in 1,2-dichloroethane (140 ml) under ice-cooling. After 30 minutes of stirring at the same temperature, sodium triacetoxyborohydride (26 g) was added by small portions to the solution over 10 minutes. After 2 hours of stirring at room temperature, the mixture was poured into a solution of sodium hydrogen carbonate (48 g) in water (300 ml). The aqueous layer was separated and adjuster to pH 12 with 24% sodium hydroxide aqueous solution. The alkaline solution was extracted with ethyl acetate 12 times. The extract was dried over sodium sulfate and evaporated under reduced pressure to give colorless crystals of 2-benzylamino-2-methyl-1-propanol (13.2 g). mp: 46.0-47.0 C. IR (Nujol): 3330, 3100, 2900, 1450, 1380, 1355 cm-1 NMR (DMSO-d6, delta): 0.99 (6H, s), 3.23 (2H, d, J=3.9Hz), 3.62 (2H, s), 4.50-4.60 (1H, m), 7.16-7.36 (5H, m)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,124-68-5, its application will become more common.

Reference:
Patent; MIYAKE, HIROSHI; TAKE, KAZUHIKO; SHIGENAGA, SHINJI; AZAMI, HIDENORI; SASAKI, HIROSHI; EIKYU, YOSHITERU; NAKAI, KAZUO; ISHIDA, JUNYA; MANABE, TAKASHI; KONISHI, NOBUKIYO; TERASAKA, TADASHI; US2003/114668; (2003); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Related Products of 2566-44-1, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 2566-44-1 as follows.

Reaction A : Dissolve oxalyl chloride (9.3 mL, 106.7 mmol) in dichloromethane (140 mL) at ambient temperature, then cool to-78C and add slowly a solution of DMSO (11.22 g, 143.6 mmol) in dichloromethane (20 mL) while venting the mixture and stir the reaction at-78C for 20 minutes. Add 2-cyclopropyl-ethanol (6.11 g, 71.21 mmol) in dichloromethane (20 mL). Warm to 0C and add dichloromethane (25 mL) to assist with stirring and mix for 30 minutes. Dilute this reaction mixture with 100 mL THF and pour into a cold (-78C) solution of Reaction B. Reaction B : Add a solution of tert-butyl acetate (62 mL, 424 mmol) in THF (60 mL) to a cold solution (-78C) of lithium diisopropylamine (2M in heptanes/tetrahydrofuran/ethylbenzene, 180 mL, 360 mmol) in anhydrous THF (700 mL) and stir at-78C for 1.5-2 hours. Add crude Reaction A prepared as described above and rinse with 100 mL anhydrous THF. Stir at-78C for 1.5 hours then add water/diethyl ether and warm to ambient temperature overnight. Separate the layers and extract the aqueous layer with diethyl ether (3x). Dry the combined organic extracts over anhydrous MgS04, filter, and concentrate in vacuo. Purify the reaction on silica gel eluting with 20% EtOAc/hexanes to give 4-cyclopropyl-3-hydroxy-butyric acid tert butyl ester (10. 65 g. 75%).’H NMR (CDC13) 6 4.11-4. 05 (m, 1H), 3. 12 (d, 1H), 2.53 (dd, 1H), 2.38 (dd, 1H), 1. 60- 1.48 (m, 1H), 1.47 (s, 9H), 1.32-1. 23 (m, 1H), 0.80-0. 73 (m, 1H), 0.51-0. 46 (m, 2H), 0. 13-0. 04 (m, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2566-44-1, its application will become more common.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/92835; (2005); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 504-63-2, name is 1,3-Propanediol, molecular formula is C3H8O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. SDS of cas: 504-63-2

General procedure: To a solution of 1,3-propanediol (19) (6.51 mL, 90 mmol) in dry DMF (40 mL) was added NaH (60% oil dispersion; 1.20 g, 30 mmol) in installments at 0 C and the mixture was stirred at room temperature for 10 min. Dodecyl bromide (4.80 mL, 20 mmol) and KI (3.32 g, 20 mmol) were added and the mixture was heated at 95 C for 4 h. After cooling, the mixture was poured into ice-water and extracted with AcOEt. The extracts were washed with brine, dried over Na2SO4 and evaporated. The resulting residue was purified by flash CC (silica gel; AcOEt/hexane, 1:2) to provide dodecyl ether 20a (3.38 g, 69%). Tetradecyl ether 20b (79%) and hexadecyl ether 20c (77%) were similarly prepared from 1,3-propanediol (19).

With the rapid development of chemical substances, we look forward to future research findings about 504-63-2.

Reference:
Article; Yamano, Yumiko; Tsuboi, Kazuhito; Hozaki, Yuki; Takahashi, Kiyohiro; Jin, Xing-Hua; Ueda, Natsuo; Wada, Akimori; Bioorganic and Medicinal Chemistry; vol. 20; 11; (2012); p. 3658 – 3665;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Application of 534-03-2, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 534-03-2, name is 2-Aminopropane-1,3-diol. A new synthetic method of this compound is introduced below.

The synthetic steps taken in this embodiment are as follows:Preparation of 5-dimethylamino-1,3-dioxan-2-one:After dissolving 19.97 g of serinol in 50 mL of formic acid, 40 mL of a 37% (w/v) formaldehyde solution was added, and the mixture was heated to 120 C for 8 hours, and then cooled to room temperature. After removing excess formic acid, formaldehyde and water from the product by a rotary evaporator, the product was evaporated to dryness with anhydrous magnesium sulfate. The filtrate was collected by filtration and subjected to distillation under reduced pressure. The fraction of 108-109 C was collected under a vacuum of 2 mbar, and crystallized at -20 C to obtain a pale intermediate in a yield of 63.6%. Characterization by infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy (1H NMR) confirmed that the pale intermediate was 2-dimethylamino-1,3-propanediol.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,534-03-2, its application will become more common.

Reference:
Patent; Guangdong Microbiology Institute (Guangdong Microbiology Analysis To Detect Center); Dong Peng; Xie Xiaobao; Gan Shuzhao; Shi Qingshan; (8 pag.)CN109467547; (2019); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 1072-52-2, 2-(Aziridin-1-yl)ethanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, 1072-52-2, blongs to alcohols-buliding-blocks compound. Computed Properties of C4H9NO

Example 20 (Scheme 15): Preparation of 2-((2-bromoethyl)-2-{ll-[2-((2-bromoethyl){2- [(methylsulfonyl)oxy] ethyl} amino)-3,5-dinitrophenyl] -6-hydroxy-6-oxido-ll-oxo-5,7- dioxa-2,10-diaza-6-phosphaundec-l-anoyl}-4,6-dinitroanilino)ethyl methanesulfonate(52); Reaction of 37 as in Scheme 15 gave 2-((2-bromoethyl)-2-{l l-[2-((2-bromoethyl){2- [(methylsulfonyl)oxy]ediyl}arnino)-3,5-dinitrophenyl]-6-oxido-ll-oxo-5,7-dioxa-2,10-diaza-6- phosphaundec-l-anoyl}-4,6-dinitroanilino)ethyl methanesulfonate (51) as a yellow oil: 1H NMR [(CDj)2SO] delta 8.99 (t, / = 5.6 Hz, 2 H), 8.75 (d, / = 2.8 Hz, 2 H), 8.40 (d, / = 2.8 Hz, 2 H), 6.98 (dj = 709 Hz, 1 H), 4.28 (t,/ = 5.5 Hz, 4 H), 4.20 (m, 4 H), 3.58 (m, 8 H), 3.48 (m, 8 H), 3.13 (s, 6 H); 13C NMR delta 165.5, 145.9, 145.3, 140.9, 135.6, 127.6, 122.4, 67.4, 63.4, 54.3, 51.1, 39.7, 36.4, 29.7; HRMS (FAB) calcd for C28H3879Br2N8O19PS2 [M+H]+ m/Z 1042.9799; found 1042.9786.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1072-52-2, its application will become more common.

Reference:
Patent; AUCKLAND UNISERVICES LIMITED; WO2008/30112; (2008); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Application of 109-83-1, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 109-83-1, name is 2-(Methylamino)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

Example 86 2-N-methyl-benzyloxycarbonylaminoethanol. To N-methylethanolamine (149 mmol) in methylene chloride (100 ml) at 0C was added benzyl chloroformate (10.0 ml, 70 mmol). The mixture was stirred at 0C for 30 min, then at room temperature for 1 h, poured into ethyl acetate, washed with 2 M HCl, saturated NaHCO3 solution, and brine, then dried over Na2SO4 and evaporated to provide 12.91 g (94%) of the desired compound. 1H NMR (CDCl3,TMS) delta 7.36 (m,5H), 5.14 (s,2H), 3.78 (m,2H), 3.47 (m,2H), 3.01(s, 3H).

According to the analysis of related databases, 109-83-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ABBOTT LABORATORIES; EP341602; (1989); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Related Products of 33420-52-9, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 33420-52-9, name is 2,2-Difluoropropan-1-ol. A new synthetic method of this compound is introduced below.

2-Chloro-6-methylpyridine-3-carbonitrile (600 mg; 3.93 mmol) in 10 mL of N,N- dimethylformamide is cooled to 0C and sodium hydride (55% in mineral oil) (429 mg; 9.83 mmol) is added to the reaction mixture. After stirring for a few minutes, 2,2-difluoropropan-1- ol (453 mg; 4.72 mmol) is added and the reaction mixture is stirred for 2 hours at 50C. The reaction mixture is quenched with methanol, filtered and purified by reverse phase chromatography-HPLC (modifier: trifluoroacetic acid) Yield: 355 mg (43 % of theory) (0309) Mass spectrometry (ESI+): m/z = 213 [M+H]+ (0310) HPLC (Method 3): Retention time = 1.020 min

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,33420-52-9, its application will become more common.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; TRIESELMANN, Thomas; GODBOUT, Cedrickx; HOENKE, Christoph; VINTONYAK, Viktor; (130 pag.)WO2019/149660; (2019); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts