Month: December 2020

100-37-8, 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. 100-37-8, name is 2-(Diethylamino)ethanol, molecular formula is C6H15NO, 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.

Example 32; N-cyclopropyl-3-({4-[(6-{ [2-(diethylamino) ethoxy] methyl} pyridin-2- yl) methoxy] benzoyl} amino)-4-methylbenzamide To a 60% dispersion of NaH in mineral oil (25 mg, 0.625 mmol) in DMA (4 mL) was added N,N-diethylethanolamine (24 mg, 0.205 mmol). The reaction was stirred at room temperature for 20 minutes. A solution of 3- [ (4- { [6- (bromomethyl) pyridin-2- yl] methoxy benzoyl) amino]-N-cyclopropyl-4-methylbenzamide (77 mg, 0.155 mmol) in DMA (2 mL) was added dropwise to the reaction which was then stirred for 1 h at room temperature. The reaction was quenched by the addition of water (1 mL) and was purified by preparative HPLC to give the title compound as a white solid (29 mg, 35%); NMR Spectrum: (DMSOd6) 0.58 (m, 2H), 0.69 (m, 2H), 0.96 (t, 6H), 2.26 (s, 3H), 2.50 (m, 4H), 2.64 (t, 2H), 2.86 (m, 1H), 3.59 (t, 2H), 4.59 (s, 2H), 5.75 (s, 2H), 7.18 (d, 2H), 7.33 (d, 1H), 7.42 (m, 2H), 7.64 (dd, 1H), 7.80 (s, 1H), 7. 87 (t, 1H), 7.96 (d, 2H), 8. 36 (d, 1H), 9.83 (s, 1H) ; Mass Spectrum : M+H+ 531.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 100-37-8, 2-(Diethylamino)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2005/61465; (2005); A1;,
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770-71-8, 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.770-71-8, name is Adamantan-1-ylmethanol, molecular formula is C11H18O, molecular weight is 166.26, as common compound, the synthetic route is as follows.

General procedure: To a solution of alcohol (1 mmol) in MeCN-H2O (9:1, 3 mL) were successively added TEMPO (7.8 mg,5 mol%), NH4OAc (0.308 g, 4 equiv), and PhI(OAc)2 (0.708g, 2.2 equiv). The suspension was stirred at roomtemperature (progress of the reaction was monitored byTLC) for the reaction time indicated in Table 2. The resultantclear two-phase reaction mixture was concentrated, dilutedwith H2O and Et2O, and the organic layer was dried (Na2SO4), filtered, and evaporated under reduced pressure.The residue was purified by flash column chromatography(PE-Et2O or PE-CH2Cl2) to give 2.

Statistics shows that 770-71-8 is playing an increasingly important role. we look forward to future research findings about Adamantan-1-ylmethanol.

Reference:
Article; Vatele, Jean-Michel; Synlett; vol. 25; 9; (2014); p. 1275 – 1278;,
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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.616-29-5, name is 1,3-Diaminopropan-2-ol, molecular formula is C3H10N2O, molecular weight is 90.12, as common compound, the synthetic route is as follows.616-29-5

Example 110; 8-r3-Bromophenyl)-3-hydroxy-8-(4-methoxvphenvD-3,4,7,8-tetrahydroimidazo[l,5- fllpvrimidine-6(2H)-thione0; 4-(3-Bromophenyl)-4-(4-methoxyphenyl)-l,3-thiazolidine-2,5-dithione (82 mg, 0.20 mmol), l,3-diaminopropan-2-ol (54 mg, 0.60 mmol) and triethylamine (139 muL, 1 mmol), was heated to 70 C in ethanol (2 mL) for 1 h. The mixture was concentrated in vacuo and the residue was diluted with ethyl acetate and washed with aqueous sodium carbonate, 0 brine, dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography using an eluent with ethyl acetate in heptane (0-100 %) to give 83 mg (96 % yield): MS (AP) m/z 433 [M+l]+.

Statistics shows that 616-29-5 is playing an increasingly important role. we look forward to future research findings about 1,3-Diaminopropan-2-ol.

Reference:
Patent; ASTRAZENECA AB; ASTEX THERAPEUTICS LTD; WO2007/145569; (2007); A1;,
Alcohol – Wikipedia,
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647-42-7, 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. 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, molecular formula is C8H5F13O, 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.

General procedure: To a stirred solution of the corresponding thiazoline 4a-c (2.0 mmol) in dry CH2Cl2 (8 mL) under N2 atmosphere at room temperature, were added subsequently the corresponding alcohol (2.0 mmol) EDCI (2.0 mmol) and catalytic amount of DMAP. After 16 h, the organic phase was transferred to an extraction funnel, washed with saturated NaHCO3 (2 ¡Á 10 mL), water (2 ¡Á 10 mL) and the organic layer was dried with Na2SO4. The solvent was evaporated and the remaining product was purified by chromatography (hexanes/AcOEt = 80:20).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 647-42-7, 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Schneider, Juliana M. F. M.; Sales, Eric S.; Livotto, Paolo R.; Schneider, Paulo H.; Merlo, Aloir A.; Journal of the Brazilian Chemical Society; vol. 25; 8; (2014); p. 1493 – 1503;,
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101-98-4, A common compound: 101-98-4, name is 2-(Benzyl(methyl)amino)ethanol,molecular formula is C10H15NO, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

A 500 mL flask (reactor flask) was charged with N-benzyl-N-methylethanolamine (24.5 mL), DCM (120 mL), NaOH (80 mL; 30 wt %) and tetrabutylammonium chloride. Mixing at low speed throughout the reaction, the mixture was cooled to -10 C. (cooling bath), and the addition funnel charged with DCM (30 mL) and mesyl chloride (15.85 mL), which was added drop wise at a constant rate over 30 minutes. The addition was exothermic, and stirring was continued for 15 minutes while the temperature equilibrated back to -10 C. The reaction was held for at least 10 minutes to ensure full hydrolysis of the excess mesyl chloride.A 250 mL flask was charged with biphenyl-2-ylcarbamic acid piperidin-4-yl ester (26 g; prepared as described in Preparation 3) and DCM (125 mL), stirred for 15 minutes at room temperature, and the mixture chilled briefly to 10 C. to form a slurry. The slurry was then charged into the reactor flask via the addition funnel. The cooling bath was removed and the reaction mixture was warmed to 5 C. The mixture was transferred to a separatory funnel, the layers allowed to settle, and the aqueous layer removed. The organic layer was transferred back to the reactor flask, stirring resumed, the mixture held to room temperature, and the reaction monitored by HPLC for a total of 3.5 hours.The reactor flask was charged with NaOH (1M solution; 100 mL), stirred, and the layers allowed to settle. The organic layer was separated, washed (NaCl saturated solution), its volume partially reduced under vacuum, and subjected to repeated IPA washings. The solids were collected and allowed to air-dry (25.85 g, 98% purity). Additional solids were obtained from further processing of the mother liquor (volume reduction, IPA, cooling).

With the rapid development of chemical substances, we look forward to future research findings about 101-98-4.

Reference:
Patent; Mu, YongQi; Dalziel, Sean M.; Ji, Yu-Hua; Preza, Leticia Maria; US2008/58374; (2008); A1;,
Alcohol – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 770-71-8, Adamantan-1-ylmethanol, 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, 770-71-8, blongs to alcohols-buliding-blocks compound. 770-71-8

Example 57A 1-(azidomethyl)tricyclo[3.3.1.13,7]decane 1-Adamantanemethanol (500 mg) was dissolved in dichloromethane (15 mL). The solution was chilled in an ice bath and triethylamine (0.587 mL) was added, followed by methanesulfonyl chloride (0.258 mL). The reaction mixture was stirred for 4 hours at 0 C., then transferred to a separatory funnel and rinsed with 1N aqueous HCl (15 mL), saturated aqueous NaHCO3 (15 mL) and brine (15 mL). The organic extracts were dried (Na2SO4), filtered, and concentrated. A portion of the resulting crude mesylate (293 mg) and sodium azide (390 mg) were combined in N,N-dimethylformamide (1.2 mL) and the reaction mixture was heated to 120 C. overnight, then cooled to room temperature and partitioned between ethyl acetate (3*15 mL) and water (20 mL). The organic extracts were dried (Na2SO4), filtered, and concentrated to provide the title compound, which was used in the next step without further purification.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,770-71-8, its application will become more common.

Reference:
Patent; AbbVie Inc.; WANG, LE; Doherty, George; Wang, Xilu; Tao, Zhi-Fu; Bruncko, Milan; Kunzer, Aaron R.; Wendt, Michael D.; Song, Xiaohong; Frey, Robin; Hansen, Todd M.; Sullivan, Gerard M.; Judd, Andrew; Souers, Andrew; US2013/96120; (2013); 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 64431-96-5, name is 2,2′-(Propane-1,3-diylbis(azanediyl))bis(2-(hydroxymethyl)propane-1,3-diol). This compound has unique chemical properties. The synthetic route is as follows. 64431-96-5

1 was prepared by the self-assembly approach: Na2MoO4¡¤2H2O (1.400g, 6.394mmol) and H6bthmap (0.414g, 1.466mmol) were dissolved in water (30mL, 1665mmol) at room temperature, and then the pH was adjusted to 4.0 with 6mol¡¤L-1 HCl. CoCl2¡¤6H2O (0.237g, 0.996mmol) and Ho(NO3)3¡¤5H2O (0.250g, 0.591mmol) were added, and then the pH was adjusted to 4.0 again with 6mol¡¤L-1 HCl. The reaction solution was stirred at ambient temperature for 30min, kept in the 70C water bath for 30min, filtered and evaporated at room temperature. Colorless block crystals were obtained after three weeks. Yield: ca. 42% (based on Na2MoO4¡¤2H2O). Anal. calcd. (found %) for C22H58Mo8N4Na2O40 (1): C 14.42 (14.63), H 3.19 (3.36), N 3.06 (2.95), Na 2.70 (2.51), Mo 41.74 (41.89). The synthetic method of 2 is similar to that of 1 except that (NH4)6Mo7O24¡¤4H2O (0.800g, 0.647mmol) substituted NaMoO4¡¤2H2O, CoCl2¡¤6H2O was replaced by CuCl2¡¤2H2O (0.400g, 2.346mmol) and the stirring time was added to 45min. Blue block crystals were obtained after two weeks. Yield: ca. 45% (based on (NH4)6Mo7O24¡¤4H2O). Anal. calcd. (found %) for C22H70 Cu2Mo8N10O38 (2): C 13.36 (13.49), H 3.57 (3.75), N 7.08 (6.91), Cu 6.22 (6.43), Mo 38.95 (38.81). Notably, albeit CoCl2¡¤6H2O and Ho(NO3)3¡¤5H2O in the preparation of 1 and Ho(NO3)3¡¤5H2O in the preparation of 2 were used as the starting materials, they can’t be observed in the products. When they were moved away under similar conditions, 1 and 2 can’t be obtained, which suggest that there are the collaborative influences of them and other reaction ingredients during the formation of 1 and 2.

Statistics shows that 64431-96-5 is playing an increasingly important role. we look forward to future research findings about 2,2′-(Propane-1,3-diylbis(azanediyl))bis(2-(hydroxymethyl)propane-1,3-diol).

Reference:
Article; Li, Hailou; Shao, Bo; Li, Yanyan; Chen, Lijuan; Zhao, Junwei; Inorganic Chemistry Communications; vol. 61; (2015); p. 68 – 72;,
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616-29-5 , The common heterocyclic compound, 616-29-5, name is 1,3-Diaminopropan-2-ol, molecular formula is C3H10N2O, 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.

Example 13 delta-CS-BromophenvD-S-hvdroxy-delta-^-methoxyphenylVS^J^-tetrahydroimidazorLS- alpyrimidine-6(2H)-thione4-(3-Bromophenyl)-4-(4-methoxyphenyl)-l,3-thiazolidine-2,5-dithione (82 mg, 0.20 mmol), l,3-diaminopropan-2-ol (54 mg, 0.60 mmol) and triethylamine (139 muL, 1 mmol), was heated to 70 C in ethanol (2 mL) for 1 h. The mixture was concentrated in vacuo and the residue was diluted with ethyl acetate and washed with aqueous sodium carbonate, brine, dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography using an eluent with ethyl acetate in heptane (0-100 %) to give 83 mg (96 % yield): MS (AP) m/z 433 [M+l]+.

According to the analysis of related databases, 616-29-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; ASTEX THERAPEUTICS LTD; WO2007/145571; (2007); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

873-63-2, 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.873-63-2, name is 3-Chlorobenzyl alcohol, molecular formula is C7H7ClO, molecular weight is 142.58, as common compound, the synthetic route is as follows.

General procedure: A 50 mL round bottom flask was charged with a mixture of aryl chloride (0.5 mmol), arylboronic acid (0.75 mmol), K2CO3 (1.5 mmol), Pd catalyst (0.2 mol %), solvent (6 mL) and the mixture was stirred for required times at appropriate temperature. After completion, the reaction mixture was diluted with water (20 mL) and extracted with ether (20 mL ¡Á3). Combined extract was washed with brine (20 mL ¡Á3) and dried over Na2SO4. After evaporation of the solvent under reduced pressure, the residue was chromatographed (silica gel, ethyl acetate/hexane 1:9) to obtain the desired product. The products were confirmed by comparing the melting points, 1H NMR and mass spectral data with authentic samples.

Statistics shows that 873-63-2 is playing an increasingly important role. we look forward to future research findings about 3-Chlorobenzyl alcohol.

Reference:
Article; Shahnaz, Nasifa; Banik, Biplab; Das, Pankaj; Tetrahedron Letters; vol. 54; 22; (2013); p. 2886 – 2889;,
Alcohol – Wikipedia,
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3360-41-6, 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 3360-41-6, name is 4-Phenylbutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

To a mixture of 5 ml (32.75 mmol) 4-phenylbutanol with 10.1 ml (65.66 mmol) 1,6-dibromohexane is added 8 g (121.2 mmol) powdered KOH and 1.112 g (3.28 mmol) tetrabutylammonium hydrogen sulfate. After allowing the suspension to stir for 20 hr at room temperature, it is filtered and the filtrate dissolved in 50 ml Et2O. The resulting solution is washed with water, dried on anhydrous Na2SO4, the Et2O evaporated and the residue distilled in vacuum (0.1 mmHg), a first fraction up to 100 C. of a mixture of starting products and a second fraction at 150 C. of 4-(6-bromohexyloxy)butylbenzene weighing 7.60 g (74.4 %) being collected. RMN 1H (CDCl3), delta (ppm): 1.3-2.0 (m, 12H), 2.6 (t, 2H, -CH2-C6H5), 3.4 (m, 6H, -CH2-O-CH2-+-CH2Br), 7.1-7.4 (m, 5H, -C6H5).

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 3360-41-6, 4-Phenylbutan-1-ol.

Reference:
Patent; Bessa Bellmunt, Jordi; Dalmases Barjoan, Pere; Marquillas Olondriz, Francisco; US6388134; (2002); B1;,
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