Tag: M.W=100-200

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 558-42-9, name is 1-Chloro-2-methyl-2-propanol. This compound has unique chemical properties. The synthetic route is as follows. 558-42-9

6-Methoxy-l’- (2-phenoxyethyl)-2, 3,4, 9-tetrahydrospiro[beta-carboline-1, 3′-pyrrolidine] (EXAMPLE 10,66 mg, 0.2 mmol, K2CO3 (48 mg, 0.3 mmol), 1-chloro-2-methylpropan-2- ol (28 mg, 0.3 mmol) and acetonitrile (2 mL) were stirred at75 C for 16h. MoreK2CO3 (48 mg, 0.3 mmol), 1-chloro-2-methylpropan-2-ol (28 mg, 0.3 mmol) were added to the reaction and1-chloro-2-methylpropan-2-ol (28 mg, 0.3 mmol) was added again after 24h and 48h. After another 72h, the mixture was filtered and the solvent was removed. The product was purified by preparative HPLC using acetonitrile-water gradients containing 0.1percent trifluoroacetic acid. Yield: 6.96 mg (8percent).HPLC 98percent, RT : 2.099 (10-97percent MeCN over 3 min). ‘H NMR (270 MHz, Methanol-d3)8 ppm 1.26 (s, 3 H) 1.35 (s, 3 H) 2.46-2. 53 (m,1 H) 2.84-3. 04 (m,1 H) 3.04-3. 14 (m, 2 H) 3. 47-3. 66 (m,6 H) 3.81 (s,3 H) 3.84 (dd,J=6. 68,3. 22 Hz, 2 H) 4.18-4. 29 (m,1 H) 4.32-4. 35 (m, 2 H) 6.81(dd,J=8. 91,2. 47 Hz, 1 H) 6.95-7. 02 (m, 4 H) 7.23-7. 33 (m,3 H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 558-42-9, 1-Chloro-2-methyl-2-propanol.

Reference:
Patent; BIOVITRUM AB; WO2005/48916; (2005); A2;,
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Adding a certain compound to certain chemical reactions, such as: 431-38-9, 3-Amino-1,1,1-trifluoropropan-2-ol, 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, 431-38-9, blongs to alcohols-buliding-blocks compound. 431-38-9

A solution of 100 mg intermediate 6, 83.2 mg 3-amino-1,1,1-trifluoropropan-2-ol, 184 mgHATU and 0.17 mL ethyldiisopropylamine in 5 mL of DMF was stirred at room temperature for14 hours. Then the reaction was quenched by water, and the mixture was extracted with dichloromethane two times. The combined organic phases were dried over sodium sulfate and evaporated to dryness. The residue was subjected to flash chromatography (dichloromethane / methanol gradient with up to 2% methanol) to yield 65mg 6-(4-methylphenyl)-2-(1-methyl-1H-pyrazol-4-yl)-3-oxo-N-(3 ,3,3-trifluoro-2-hydroxypropyl)-2 ,3-dihydropyridazi ne-4-carboxamide.1H-NMR (400 MHz, CDCI3): 6 [ppm] = 2.44 (s, 3H); 3.78 (ddd, 1H); 3.90 (ddd, 1H); 3.99 (s,3H); 4.18-4.27 (m, 1H); 4.56 (d, 1H); 7.33 (d, 2H); 7.82 (d, 2H); 8.16 (s, 1H); 8.33 (s, 1H); 8.71(s, 1H); 10.24 (bt, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,431-38-9, its application will become more common.

Reference:
Patent; BAYER AKTIENGESELLSCHAFT; BAYER PHARMA AKTIENGESELLSCHAFT; DEUTSCHES KREBSFORSCHUNGSZENTRUM; GUTCHER, Ilona; ROeHN, Ulrike; SCHMEES, Norbert; ZORN, Ludwig; ROeSE, Lars; BADER, Benjamin; KOBER, Christina; CARRETERO, Rafael; STOeCKIGT, Detlef; IRLBACHER, Horst; PLATTEN, Michael; (397 pag.)WO2018/146010; (2018); A1;,
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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 624-95-3, name is 3,3-Dimethylbutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows. 624-95-3

Example IV represents an oxidation in which the KBr co-catalyst and the NaHCO3 buffer were removed and replaced with Na2B4O7 additive. [00065] 16.9 g of 3,3-Dimethyl-1-butanol (117.3 mmol) and 0.0765 g MeO-TEMPO (0.411 mmol) are charged in a jacketed glass reaction flask as in Example I. Sodium borate (0.380 g, 1.0 mmol) is dissolved in water (12.0 cc) and the aqueous solution is added to the stirred organic fraction at 1000 RPM in the reaction flask. The stirred suspension is cooled to 0 C. and the emulsion is re-adjusted to pH=8.4 using 50% solution of CH3COOH. When the temperature of the reactants reached 0 C., 75.5 g (122 mmol) of 12.1% aqueous NaOCl solution are pumped in via a gas-tight syringe over 90 minutes. During the bleach addition, the pH was maintained at 8.3-8.4 levels using a few drops of 50% aqueous CH3COOH. The reaction mixture is stirred for an additional 120 min at 0 C. and the organic layer is sampled for GC assay. The reaction in this second stage was kept at pH 8.4 by addition of 0.2-0.25 cc aqueous solution of NaOH (50% concentration). The yield of 3,3-dimethylbutyraldehyde is 90.0% at 60 min and 91.0% at 90 min reaction time

Statistics shows that 624-95-3 is playing an increasingly important role. we look forward to future research findings about 3,3-Dimethylbutan-1-ol.

Reference:
Patent; The NutraSweet Company; US6825384; (2004); B1;,
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100-37-8 , The common heterocyclic compound, 100-37-8, name is 2-(Diethylamino)ethanol, molecular formula is C6H15NO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

(1) Synthesis: 240 g (2.4 mol) of methyl methacrylate,117 g (1.0 mol) of diethylaminoethanol, 200 g of n-hexane,8 g of lithium hydroxide and 0.5 g of phenothiazine were added with stirring,Thermometer and water separator in a 1000 mL three-necked flask,Heated to 65 C ~ 73 C, constantly reflux and separation of methanol,The reaction was stopped (about 5 h) after refluxing to the absence of methanol separation.34.5 g of methanol was separated,Gas chromatographic analysis showed that the methanol content was 88.6%The methyl methacrylate content was 11.2%.(2) purification: cooling to room temperature, add 300mL ¡Á 2 of deionized water washed twice. The oil was gradually decompressed (0 to 100 mmHg) at 60 C to 100 C,Unreacted methyl methacrylate and diethylaminoethanol,And then diethyl etherate methacrylate was distilled off under reduced pressure at 5 to 10 mmHg and 90C to 100C. The resulting product was 175.7 g (theoretical yield 185.26 g) in a yield of 94.1%.Gas chromatographic analysis showed that the content of diethylaminoethyl methacrylate was99.2%.

According to the analysis of related databases, 100-37-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Qingdao University of Science and Technology; Tang Linsheng; Yang Jingwei; Wu Hongzhi; Hou Xiaomin; Zhu Xin; Mi Chengjing; (9 pag.)CN106966913; (2017); A;,
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108-82-7, 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 108-82-7, name is 2,6-Dimethylheptan-4-ol. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: NaOCl¡¤5H2O crystals (2.0 g, 12.2 mmol) were added in oneportion to a mixture of Bu4NHSO4 (0.17 g, 0.50 mmol),TEMPO (21 mg, 0.13 mmol), and 1 (1.30 g, 10.0 mmol) inCH2Cl2 (10 mL) at 5 C. After 15 min, GC monitoringshowed that 1 had been consumed. The reaction was stoppedafter 0.5 h by quenching with aq sat. Na2SO3 solution (20mL). The organic layer was separated, and the aqueous layerwas extracted with CH2Cl2 (30 mL). The combined organiclayers were washed with H2O (30 mL), dried over Na2SO4,and concentrated to give 2 as colorless oil (1.27 g, crudeyield of 99.2%, GC analysis showed the product to be 96.8%pure). A 0.42 g portion of the crude 2 was purified by bulbto-bulb distillation (6 kPa, 120-130 C) to afford pure 2(0.40 g, 95%). GC-MS analysis gave identical results tothose of an authentic sample.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 108-82-7, 2,6-Dimethylheptan-4-ol.

Reference:
Article; Okada, Tomohide; Asawa, Tomotake; Sugiyama, Yukihiro; Kirihara, Masayuki; Iwai, Toshiaki; Kimura, Yoshikazu; Synlett; vol. 25; 4; (2014); p. 596 – 598;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 702-82-9, name is 3-Aminoadamantan-1-ol. This compound has unique chemical properties. The synthetic route is as follows. 702-82-9

General procedure: For compounds 9-13, a mixture of 77-155mg (0.6-1.2mmol) of phthaldialdehyde 8 and equal molar amount of appropriately substituted adamantylamine or noradamantylamine (if utilized as the hydrochloride salt, potassium carbonate, 0.55-1.0eq, was added as appropriate) in 40-80mL tetrahydrofuran was stirred for 171.5-211.0h under a nitrogen atmosphere at room temperature. After removing solvent, the residues were purified by silica gel chromatography (EtOAc/Hex or MeOH/CH2Cl2)

At the same time, in my other blogs, there are other synthetic methods of this type of compound,702-82-9, 3-Aminoadamantan-1-ol, and friends who are interested can also refer to it.

Reference:
Article; Luo, Weiming; Tweedie, David; Beedie, Shaunna L.; Vargesson, Neil; Figg, William D.; Greig, Nigel H.; Scerba, Michael T.; Bioorganic and Medicinal Chemistry; vol. 26; 8; (2018); p. 1547 – 1559;,
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627-18-9, 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 627-18-9, name is 3-Bromopropan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

Take a 500 mL three-necked flask dried in an oven, equipped with a mechanical stirrer and a thermometer. Add 98% sulfuric acid (50.0 g, 0.5 mol), dichloromethane 60 mL, and cool to -5 to 5 C in an ice salt bath. Fuming nitric acid (33.5g, 0.5mol) was slowly added. Then, 3-bromo-1-propanol (46 g, 0.33 mol) was added dropwise to the mixture, and the reaction medium was stirred at -5 to 5 C for 4 to 5 hours. The mixture was poured into cold water (350 g) maintaining the temperature between -5 and 5 C. After pouring, the organic phase was taken, 80 mL of dichloromethane was added to the aqueous phase, the organic phase was combined, the combined organic phases were washed with water, adjusted to pH = 6-7 by adding 8% sodium hydroxide, washed with brine, organic phase Dry with magnesium sulfate. Dichloromethane was evaporated under reduced pressure to give 3-bromopropyl nitrate (yield compound of formula M) (53.5 g, 88.1%).

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 627-18-9, 3-Bromopropan-1-ol.

Reference:
Patent; Chongqing Weipeng Pharmaceutical Co., Ltd.; Li Nenggang; Liu Zeyan; Lin Song; Chen Xiaopeng; Zhou Xingguo; Yao Hequan; (18 pag.)CN108892624; (2018); A;,
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1462-03-9 ,Some common heterocyclic compound, 1462-03-9, molecular formula is C6H12O, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

Preparation 8; 1-Methvl-cvclopentvlamine hvdrochloride; A solution of 2.00 g (20 mmol) of 1-methylcyclopentanol in 25 mL of benzene was treated with 3.18 mL (24 mmol) of azidotrimethylsilane and 3.04 mL (24 mmol) of boron trifluoride etherate as described by Zwierzak, et al., Tetrahedron Letters, 1987, 6513. After about 24 hrs, the solution was poured into 50 mL of 1 M sodium bicarbonate solution and stirred for 30 minutes, adding solid sodium bicarbonate as needed to maintain pH > 7. The benzene layer was separated and dried over anhydrous calcium chloride. The benzene solution was diluted with 25 mL of methanol hydrogenated over 0.45 g of 10% Pd/C catalyst for 90 minutes at 45 psi and 20 C. The reaction mixture was then filtered through diatomaceous earth, 1.7 mL of 12 M hydrochloric acid was added to the filtrate, and the solvent was evaporated to provide 1.92 g (71%) of the title compound as a white solid. NMR (D2O) : 1.59 (m, 8 H); 1.22 (s, 3 H). APCI MS: 100 (MH+). mp: 261-262 C.

According to the analysis of related databases, 1462-03-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PFIZER PRODUCTS INC.; WO2005/95339; (2005); A1;,
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Adding a certain compound to certain chemical reactions, such as: 440-60-8, (Perfluorophenyl)methanol, 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, 440-60-8, blongs to alcohols-buliding-blocks compound. 440-60-8

EXAMPLE 1 This Example illustrates the preparation of 2-methyl-3,4,5,6-tetrafluorobenzyl alcohol. A solution of methyl bromide (9.6 g) in dry tetrahydrofuran (25 cm3) was added dropwise in a stirred mixture of magnesium turnings (5.0 g), dry tetrahydrofuran (50 cm3) and a small crystal of iodine at the ambient temperature (ca. 22 C.). When the addition was complete the mixture was stirred for a further 1 hour at the ambient temperature and the solution of methyl magnesium bromide thus formed was then added dropwise to a stirred solution to pentafluorobenzyl alcohol (17.8 g) in tetrahydrofuran (50 cm3) whilst the temperature was maintained at 30 C. When the addition was complete the mixture was stirred for a further 2 hours at the ambient temperature and for 3 hours at the reflux temperature. Water at 0 C. was added to the mixture, which was then acidified with dilute hydrochloric acid and extracted with diethyl ether (2*80 cm3). The extracts were combined, washed with water, dried over anhydrous magnesium sulphate and concentrated by evaporation of the solvent under reduced pressure. The residual oil (4.6 g) was shown by gas liquid chromatographic examination of a sample to consist of ca. 70% by weight of unreacted starting material and ca. 30% by weight of product. The oil was subjected to vigorous purification by column and thin-layer chromatography using a silica gel support and eluding with a mixture of diethyl ether and hexane (3:7 by volume), to obtain 2-methyl-3,4,5,6-tetrafluorobenzyl alcohol as a colourless oil. 1 H nmr (CDCl3) delta: 1.86 (broad s,1H); 2.35 (q,3H); 4.74 (d,2H). 19 F nmr (CDCl3) delta: -142.3 (dd, J=12.6, 21Hz); -145.9 (dd, J=12.6, 21Hz); -157.25 (t,J=21Hz); -160.5 (t,J=21Hz);

With the rapid development of chemical substances, we look forward to future research findings about 440-60-8.

Reference:
Patent; Imperial Chemical Industries PLC; US4714790; (1987); A;,
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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 624-95-3 as follows., 624-95-3

2.24 g (51.3 mmol) of 55 wt% sodium hydride was suspended in 100 ml of tetrahydrofuran. 4.24 g (41.5 mmol) of 3,3-dimethylbutanol was added dropwise to the suspension under ice cooling, and the mixture was stirred at room temperature for 15 minutes. To this was added dropwise 20 ml of a tetrahydrofuran solution of 5.0 g (37.7 mmol) of 2-chloro-5-fluoropyrimidine, followed by stirring at room temperature overnight. A saturated aqueous solution of ammonium chloride was added thereto, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and the inorganic matter was removed by filtration. The filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 4.40 g (22.2 mmol, yield 59%) of 2- (3,3-dimethylbutoxy) -5-fluoropyrimidine.

The chemical industry reduces the impact on the environment during synthesis 624-95-3, I believe this compound will play a more active role in future production and life.

Reference:
Patent; NIPPON SODA COMPANY LIMITED; ITO, SYUICHI; AMANO, TOMOHIRO; IPPOSHI, JUNJI; KOUBORI, SHINYA; (44 pag.)JP2016/30742; (2016); A;,
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