Month: June 2021

Synthetic Route of 25574-11-2, 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 25574-11-2, name is 3-(4-Bromophenyl)propan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 100. Synthesis of l-Broiotatio-4-(3-Bromo-Propyl)-Benzene (Intermediate50150[02981 To a solution of intermediate 49 (Example 99) (4.0 g, 19 mmol) in THF (30 mL)O at 0 C under the argon atmosphere was added PPh3 (6.3 g, 24 mmol) followed by CBr4 (8.0 g, 24 mmol). The mixture was stirred at the same temperature for 15 min and then stirred at room temperature for additional 15 h. Most of the solvent was removed and the residue purified by flash chromatography on silica gel (hexane) to afford the title compound (3.5 g, 66%) as a colorless oil.[0299] 1H NMR (500 MHz, DMSOd6): delta 2.03-2.12 (m, 2H), 2.68 (t, J= 7.5 Hz, 2H), 3.49 (t, J= 6.5 Hz, 2H), 7.19 (d, J= 8.3 Hz, 2H), 7.47 (d, J= 8.3 Hz, 2H).

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 25574-11-2, 3-(4-Bromophenyl)propan-1-ol.

Reference:
Patent; TARGEGEN, INC.; WO2008/8234; (2008); A1;,
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Application of 100-37-8 ,Some common heterocyclic compound, 100-37-8, 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.

Add 146g of thionyl chloride and 240g of dichloromethane to the 1L reaction bottle to cool down, use 500ml beaker during cooling processA mixed solution of 120 g of diethylaminoethanol and 100 g of dichloromethane was prepared. When the temperature in the reaction flask was lowered to -10 C, a mixture of diethylaminoethanol and dichloromethane was added dropwise at a temperature of -10 to 20 C. 1 hour and 28 minutes, the addition is completed;After the completion of the dropwise addition, the temperature was raised to 20 to 45 C for 5 hours, and after the completion of the incubation, the dichloromethane was concentrated for 1 hour and 05 minutes.Concentrated to a total of 258g of dichloromethane, the recovery of dichloromethane can be directly applied;After concentration and drying, the temperature was lowered to 27 C. 240 g of absolute ethanol was added to the reaction flask and heated to dissolve the solid.After dissolving, the ice brine was cooled to -5 to -10 C for 6 hours, and filtered to obtain 2-diethylaminochloroethane hydrochloride wet product 177.6 g wet.Product.After the mother liquor is collected, 208g of ethanol is concentrated and recovered. The recovered ethanol can be continuously applied, and the residual liquid is placed in a freezer for freezing and crystallization. After hourly filtration, 18.5 g of the mother liquor product was obtained, and then recrystallized from 32 g of recovered ethanol to obtain 13.8 g of a qualified mother liquor. A total of 191.4 g of the combined product was dried at 55-60 C to obtain 173.9 g of dry product of 2-(diethylamino)ethyl chloride hydrochloride, and the liquid phase purity was 99.82%, and the molar yield was calculated to be 98.7%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,100-37-8, its application will become more common.

Reference:
Patent; Shandong Cheng Hui Shuang Da Pharmaceutical Co., Ltd.; Wang Yongguang; Liu Xuewen; Xue Qimeng; Zhao Zhonggui; Xu Linjie; (9 pag.)CN108084033; (2018); A;,
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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. 23147-58-2, name is Glycerol aldehyde dimer, molecular formula is C4H8O4, 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. Formula: C4H8O4

To a solution of 4 (0.038 g, 0.094 mmol) in MeOH (5 mL) were added AcOH (0.108mL, 1.88 mmol, 20.0 equiv), NaBH3CN (0.018 g, 0.282 mmol, 3.0 equiv) and glycolaldehyde dimer (0.017 g, 0.141 mmol, 1.5 equiv). The reaction was warmed to 60 C and stirred for 2 hours, after which TLC analysis (CH2Cl2/MeOH/NH4OH84:15:1) showed full conversion of the starting material. The reaction mixture was concentrated in vacuo, the residue dissolved in MeOH, absorbed onto celite and purified by flash column chromatography (CH2Cl2/MeOH/NH4OH 99:0:1 to 79:20:1) to afford 3a (39 mg, 0.087 mmol, 93% yield) as a white solid.

With the rapid development of chemical substances, we look forward to future research findings about 23147-58-2.

Reference:
Article; Bouton, Jakob; Van Hecke, Kristof; Rasooly, Reuven; Van Calenbergh, Serge; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 2822 – 2828;,
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Adding a certain compound to certain chemical reactions, such as: 64372-62-9, 2-Chloro-5-(trifluoromethyl)benzyl alcohol, 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, SDS of cas: 64372-62-9, blongs to alcohols-buliding-blocks compound. SDS of cas: 64372-62-9

General procedure: A 3 M K2CO3 solution is prepared by adding solid K2C03 (31 g, 0.22 mol) to water (100 mL). Cooling is applied to keep the solution at 20-25 C. (2-chloro-5-(trifluoromethyl)phenyl)methanol (Formula VI’, X = CI, Ri = CH2OH) (17.5 g, 84 mmol), and 4-fluoro-5-isopropyl-2-methoxyphenylboronic acid (MIPB) (18.1 g, 85 mmol) are added to the K2CO3 followed by all THF (100 mL) rinse. The solution is degassed by sparging with argon gas for 20 min. The catalyst, 1 , 1-bis(di-tertbutylphosphino)ferrocene palladium dichloride (300 mg, 0.55 mol%) is added. The organic layer turns dark brown immediately. The biphasic mixture is aged at 35-45 C with vigorous stirring for 32 hours. The mixture is cooled to r. t. and water (150 mL) is added, followed by petrol ether (150 mL) and the aqueous layer is removed. The organic layer was washed with water (2×200 mL) and filtered through silica gel and the solvent is removed under reduced pressure to yield brownish oil which is crystallized from heptane to give 4′-fluoro-5′-isopropyl-2′-methoxy-4-(tnfluoromethyl)biphenyl-2-yl)methanol as a pale white solid (28.5 g, 80%). mp 93.5-95.5 C; 1H NMR (CDC ) C 1 .24 (d, J = 6.9 Hz, 6H), 1.95 (t, J = 6.1 Hz, 1 H), 3.21 (sept., J = 6.9 Hz, 1 H), 3.73 (S, 3H), 4.49 (m, 2H), 6.68 (d, J = 12.0 Hz, 1 H), 6 99 (d, J = 8.6 Hz, 1 H), 7.30 (d, J = 7.9 Hz, 1 H), 7.59 (dd, J, = 8.0 Hz, J2 = 1 .3 Hz, 1 H), 7.86 (d, J = 0.7 Hz, 1 H). According to the same procedure in various scales and different concentrations of catalyst some other biaryl of Formula VII1 and Vll2 are prepared and listed in Table 1 and Table 2, respectively.

The synthetic route of 64372-62-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LEK PHARMACEUTICALS D.D.; HUMLJAN, Jan; MARAS, Nenad; WO2013/91696; (2013); A1;,
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Reference of 109-83-1, 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 109-83-1 as follows.

To a solution of 2,6-dibromobenzaldehyde (12 g, 45.5 mmol) in MeOH (120 mL)was added NaBH4 (1.89 g, 50.0 mmol) portionwise.The mixture was stirred at roomtemperature for 1 h, quenched slowly with sat. NH4C1, and extracted with EtOAc. The combined organics were washed with brine, dried over Na2SO4 and concentrated to give the title compound. ?H NMR (400 MHz, CDC13) oe 7.55 (d, J= 7.9 Hz, 1H), 7.02 (t, J= 7.9 Hz, 1H), 5.00 (d, J 6.6 Hz, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,109-83-1, its application will become more common.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ZHANG, Hongjun; BARR, Kenneth, Jay; LAPOINTE, Blair, T.; GUNAYDIN, Hakan; LIU, Kun; TROTTER, B., Wesley; (67 pag.)WO2017/75185; (2017); A1;,
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Adding a certain compound to certain chemical reactions, such as: 13330-96-6, 4-(Dimethylamino)butan-1-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, 13330-96-6, blongs to alcohols-buliding-blocks compound. Formula: C6H15NO

General procedure: To a solution of 6-substituted pyridazinone 9 (0.5 mmol) in DMF (10 mL) was added Cs2CO3 (0.55 mmol). An appropriately substituted nitro benzyl chloride (0.52 mmol) was added and the resulting mixture was stirred at 40-50 C for 3 h, the solvent was removed under reduced pressure and the residue was dissolved in EtOAc (30 mL), which was then washed with brine (3 × 10 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated in vacuo. The crude product, 2-nitrobenzyl-6-substituted-pyridazin-3(2H)-one (10), was used in the next step without further purification. To a solution of 10 in 95 % ethanol (50 mL) was added acetic acid (10 mmol) followed by slow addition of iron powder (2 mmol). The resulting mixture was stirred for 5 h at 100 C. The mixture was then filtered through celite and the filter cake was washed with 95 % ethanol (3 × 15 mL). The combined ethanol filtrates were evaporated in vacuo and the residue was re-dissolved in ethyl acetate (30 mL). The organic layer was washed with brine (3 × 10 mL) and 2 M NaOH (10 mL) sequentially. The organic layer was dried over anhydrous Na2SO4, evaporated in vacuo to afford 2-aminobenzyl-6-substituted-pyridazin-3(2H)-one (11) as a yellow solid, which was used without further purification. To a stirred solution of 11 and triphosgene (1 mmol) in dry dichloromethane (5 mL) was added triethylamine (2 mmol) under nitrogen atmosphere. A solution of the corresponding alcohol (1 mmol) in dichloromethane (5 mL) was added 5-10 min later and the mixture was stirred at room temperature overnight, diluted with dichloromethane (15 mL) and washed with water (3 × 20 mL). The organic phases were separated, combined, dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by using column chromatography to afford the corresponding product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,13330-96-6, its application will become more common.

Reference:
Article; Xing, Weiqiang; Ai, Jing; Jin, Shiyu; Shi, Zhangxing; Peng, Xia; Wang, Lang; Ji, Yinchun; Lu, Dong; Liu, Yang; Geng, Meiyu; Hu, Youhong; European Journal of Medicinal Chemistry; vol. 95; (2015); p. 302 – 312;,
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Reference of 115-20-8, Adding some certain compound to certain chemical reactions, such as: 115-20-8, name is Trichloroethanol,molecular formula is C2H3Cl3O, 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 115-20-8.

Example 1 Preparation of intermediate 2, 2, 2-trichloroethyl 4-bromobutyrate A stirred solution of 4-bromobutyric acid (3.34 g, 20.0 mmol) in toluene (50 ml) was added 2,2, 2-trichloroethanol (14.94 g, 0.10 mol) and p-toluenesulfonic acid monohydrate (7.60 g, 40.0 mmol) and refluxed with a Dean-Stark trap attached for 6 h. Water was removed continuously. The reaction mixture was cooled to room temperature and concentrated in vacuo. The mixture was added CH2CI2 (75 ml) and washed with H2O (3 x 25 ml). The organic layer was dried over Na2SO4, filtered and evaporated in vacuo to leave an oil. The residue was distilled to leave the title compound as a colourless oil (4.77 g, 79.9 %) (bp 100 C at 0.5 mmHg). tH-NMR (300 MHz, CDCl3) : 5 4.74 (s, 2H), 3.48 (t, 2 H), 2.65 (t, 2 H), 2.21-2. 13 (m, 2 H)

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. 115-20-8, Trichloroethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BIO-MEDISINSK INNOVASJON AS; WO2005/61483; (2005); A2;,
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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. 111-32-0, name is 4-Methoxybutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows. SDS of cas: 111-32-0

Preparation 14 4-Methoxybutyl 4-bromobenzenesulfonate To a solution of 4-methoxy-1-butanol (2.0 g, 19.2 mmol) in dichloromethane (20 mL) was added triethylamine (3.9 mL, 28.9 mmol) followed by 4-bromobenzenesulfonyl chloride (7.35 g, 28.9 mmol) and the reaction mixture was stirred overnight. Hydrochloric acid (20 mL of 2 N) was added and the aqueous phase washed with dichloromethane (2 x 10 mL). The combined organic layers were washed successively with aqueous saturated sodium hydrogencarbonate (20 mL) and then water(20 mL) and then dried over MgSO4and concentrated in vacuo.The product was obtained as a pale oil (6.10 g, 98%). NMR (CDCl3): 1.6 (m, 2H), 1.8 (m, 2H), 3.3 (s, 3H), 3.35 (m, 2H), 4.1 (m, 2H), 7.6-7.9 (m, 4H).

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, 111-32-0, 4-Methoxybutan-1-ol.

Reference:
Patent; PFIZER INC.; Pfizer Limited; EP1072601; (2001); A2;,
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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.10160-24-4, name is 7-Bromo-1-heptanol, molecular formula is C7H15BrO, molecular weight is 195.0974, as common compound, the synthetic route is as follows.Recommanded Product: 7-Bromo-1-heptanol

Add 8.4 g (0.1 mol) of methyl propiolate to a 100 mL single-mouth bottle. 30 mL of dry tetrahydrofuran and 4.5 g of gram (0.115 mol) sodium amide, and the mixture was stirred at room temperature for about 15 minutes. then 21.34 g (0.11 mol) of 7-bromoheptanol was added dropwise. after 0.5 h of dropwise addition, the reaction was continued for 3.0 h. After the completion of the reaction, the tetrahydrofuran was removed in vacuo, and the residue was dissolved in dichloromethane, washed with water, and then evaporated. the filtrate was evaporated to give a pale yellow oily liquid product II compound 19.2 g, yield 97%

At the same time, in my other blogs, there are other synthetic methods of this type of compound,10160-24-4, 7-Bromo-1-heptanol, and friends who are interested can also refer to it.

Reference:
Patent; Jiaxing College; Li Meng; Zong Qianshou; Liu Xuejun; Wang Lu; Dai Jingjing; Zhang Yajing; Zheng Yannan; Zhou Hongwei; Bao Lin; (7 pag.)CN109942397; (2019); A;,
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Application of 15852-73-0, 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. 15852-73-0, name is (3-Bromophenyl)methanol. A new synthetic method of this compound is introduced below.

Preparation of [ (3-BROMOBENZYL) OXYL (TERT- butyl) dimethylsilane 232 mg (1.24 mmol) of 3-bromo-benzylalcohol was dissolved in 50 ml of methylene chloride, and 126 mg (1.85 mmol) of imidazole and 224 mg (1.49 mmol) of tert-butyldimethylsilyl chloride were added thereto, followed by stirring at room temperature. After 2 hours, a resulting white solid was filtered off, and the remaining organic layer was washed with 20 ml of 1 N aqueous hydrochloric acid and 20 ml of saturated aqueous NaCl, then dried over anhydrous MGS04. Removal of solvent in vacuo provided 306 mg (1.02 mmol) of the title compound at 82.3% yield. 1H NMR (CDCL3, PPM) ; 6 7.37 (1H, s), 7.26 (1H, d), 7.13 (1H, d), 7.08 (1H, q) FAB MS (m/e) = 302 [M+1]

At the same time, in my other blogs, there are other synthetic methods of this type of compound,15852-73-0, (3-Bromophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; LG LIFE SCIENCES LTD.; WO2004/80979; (2004); A1;,
Alcohol – Wikipedia,
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