Month: May 2021

Adding a certain compound to certain chemical reactions, such as: 616-29-5, 1,3-Diaminopropan-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, 616-29-5, blongs to alcohols-buliding-blocks compound. Product Details of 616-29-5

Step 1 : Di-tert-butyl (2-hydroxypropane-l,3-diyl)dicarbamate [00217] A solution of l,3-diaminopropan-2-ol (3.0 g, 33.3 mmol) in water (7 mL) was added to a solution of di-tert-butyldicarbonate (16.0 g, 73.7 mmol) in dioxane (400 mL). The reaction mixture was stirred for 22 h at room temperature then concentrated in vacuo. The resulting solid was dissolved in CH2C12 (300 mL), washed with water (300 mL), and dried (MgS04). Concentration in vacuo gave di-tert-butyl (2-hydroxypropane-l,3- diyl)dicarbamate (9.0 g) as a faint-yellow oil, which was used without further purification. 1H NMR (300 MHz, CDC13) delta 5.09 (br, 2H), 3.78-3.73 (m, 1H), 3.55 (br, 1H), 3.34-3.12 (m, 4H), 1.46 (s, 18H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,616-29-5, its application will become more common.

Reference:
Patent; PRESAGE BIOSCIENCES, INC.; DECKWERTH, Thomas; KLEINMAN, Edward; RUAN, Fuqiang; BAKER, William; KLINGHOFFER, Richard; (126 pag.)WO2016/196393; (2016); A2;,
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Application of 2807-30-9, 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 2807-30-9, name is 2-Propoxyethanol. This compound has unique chemical properties. The synthetic route is as follows.

Step 1: Synthesis of intermediate 3 a shown by formula (3 a); [Show Image] A four-necked reactor equipped with a condenser, a thermometer, and a dropping funnel was charged with 15 g (0.09 mol) of 5-formylsalicylic acid, 28.1 g (0.27 mol) of ethylene glycol monopropyl ether, 1.7 g (0.009 mol) of p-toluenesulfonic acid monohydrate, and 1000 ml of toluene under a nitrogen stream to prepare a homogenous solution. The solution was stirred for eight hours under reflux. Water produced during the reaction was removed together with toluene by azeotropic dehydration while adding toluene. After completion of the reaction, the reaction mixture was washed with water. After drying the toluene layer over anhydrous magnesium sulfate, magnesium sulfate was filtered off. Toluene was evaporated from the filtrate under reduced pressure to obtain a yellow oil. The yellow oil was purified by silica gel column chromatography (n-hexane:THF=3:1) to obtain 12.6 g of a light yellow solid intermediate 3a (yield: 55.5%). The structure of the intermediate 3a was identified by 1H-NMR. 1H-NMR (400 MHz, CDCl3, TMS, delta ppm): 11.34 (s, 1H), 9.89 (s, 1H), 8.42 (d, 1H, J=2.0 Hz), 8.01 (dd, 1H, J=2.0 Hz, J=8.6 Hz), 7.11 (d, 1H, J=8.6 Hz), 4.56 (t, 2H, J=4.6), 3.80 (t, 2H, J=4.6 Hz), 3.49 (t, 2H, J=6.6 Hz), 1.68-1.59 (m, 2H), 0.94 (t, 3H, J=7.6 Hz)

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 2807-30-9, 2-Propoxyethanol.

Reference:
Patent; Zeon Corporation; EP2143710; (2010); A1;,
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Related Products of 769-30-2, 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. 769-30-2, name is Benzo[d][1,3]dioxol-4-ylmethanol. A new synthetic method of this compound is introduced below.

To a solution of 4-hydroxymethyl-benzo[1 ,3]dioxole (1.00 g, 6.6 mmol) and carbon tetrabromide (3.50 g, 10.5 mmol) in anhydrous tetrahydrofuran (30 ml.) was added at 00C triphenylphosphine (2.80 g, 10.5 mmol) in solution in tetrahydrofuran (10 mL). The resulting reaction mixture was stirred at room temperature for 2 hours. Water (30 mL) was added followed by ethyl acetate (30 mL). The organic layer was washed first with a concentrated aqueous sodium hydrogenocarbonate solution (30 mL) and then brine (30 mL), dried over anhydrous potassium carbonate and concentrated in vacuum. The resulting crude product was purified by flash chromatography on silica gel, eluting with cyclohexane – dichloromethane (7:3) to afford the title compound (1.23 g, 87%) as colorless oil.[00694] 1H NMR (CDCI3): delta 6.86 – 6.75 (m, 3H), 6.02 (s, 2H), 4.47 (s, 2H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,769-30-2, Benzo[d][1,3]dioxol-4-ylmethanol, and friends who are interested can also refer to it.

Reference:
Patent; NPS PHARMACEUTICALS, INC.; WO2007/44796; (2007); A2;,
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Related Products of 15852-73-0, 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 15852-73-0 as follows.

General procedure: OMS-2-SH-B (20 mg, 10 mol%), benzyl alcohol (0.3 mmol) and benzamidine (0.5 mmol) were added into a Schlenk tube. Then, air was removed and toluene (1 mL) was added by a syringe under O2 atmosphere. If substituted benzyl alcohol was liquid, it was added with toluene under O2 balloon protection. If methyl benzene was used as substrate instead of benzyl alcohol, it was added as solvent (1 mL) into the reaction tube by syringe under O2 atmosphere. The mixture was stirred for required time at certain temperature for 20 h. The resulting mixture was cooled down, filtered and washed with EtOAc, and concentrated under reduced pressure to give the crude product. Finally, the product was purified by silica gel chromatography to yield the pure product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,15852-73-0, its application will become more common.

Reference:
Article; Shen, Jian; Meng, Xu; Catalysis Communications; vol. 127; (2019); p. 58 – 63;,
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Application of 28539-02-8, Adding some certain compound to certain chemical reactions, such as: 28539-02-8, name is 1-(Hydroxymethyl)benzotriazole,molecular formula is C7H7N3O, 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 28539-02-8.

Step A: To a mixture of 5a (0.44 g, 2.0 mmol) and EtOH (9.0 mL)was added 1H-benzotriazole-1-methanol (0.30 g, 2.0 mmol). After stirring at room temperature overnight, the reaction mixture was concentrated in vacuo and the obtained residue was triturated with hexane. The resulting precipitate was collected by filtration to give N-(1H-Benzotriazol-1-ylmethyl)-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (0.59 g, 84%) as a brown solid. 1HNMR (CDCl3) d: 8.03 (1H, d, J = 8.2 Hz), 7.67 (1H, d, J = 8.2 Hz),7.62 (1H, dd, J = 7.4, 1.6 Hz), 7.44-7.40 (1H, m), 7.33-7.28 (2H,m), 7.09 (1H, t, J = 7.2 Hz), 7.02 (1H, d, J = 8.2 Hz), 6.73 (1H, td,J = 7.4, 0.8 Hz), 6.16 (2H, d, J = 7.4 Hz), 1.37 (12H, s). MS (ESI-) m/z:349 (MH).

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. 28539-02-8, 1-(Hydroxymethyl)benzotriazole, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ogiyama, Tomoko; Yamaguchi, Mitsuhiro; Kurikawa, Nobuya; Honzumi, Shoko; Yamamoto, Yuka; Sugiyama, Daisuke; Takakusa, Hideo; Inoue, Shin-ichi; Bioorganic and Medicinal Chemistry; vol. 25; 7; (2017); p. 2234 – 2243;,
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Adding a certain compound to certain chemical reactions, such as: 15852-73-0, (3-Bromophenyl)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, 15852-73-0, blongs to alcohols-buliding-blocks compound. Formula: C7H7BrO

To a solution of 3-bromobenzyl alcohol (3.00 g, 16.0 mmol) and triethylamine (2.91 mL, 20.9 mmol) indichloromethane (50 mL) at 0 °C was added methanesulfonyl chloride drop-wise. After 2 h, the reaction mixture was washed with saturated aqueous sodium bicarbonate solution and water. The organic layer was dried over magnesium sulfate, filtered, and concentrated under reduced pressure to afford the title compound as a light yellow oil.Yield: 4.3 g, 16 mmol, 100percent. 1H NMR (400 MHz, CDCI3) oe 2.99 (5, 3H), 5.21 (5, 2H),7.30 (dd, J=7.8, 7.7 Hz, 1 H), 7.34-7.38 (m, 1 H), 7.52-7.56 (m, 1 H), 7.57-7.59 (m, 1 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,15852-73-0, its application will become more common.

Reference:
Patent; PFIZER INC.; PETTERSSON, Martin Youngjin; JOHNSON, Douglas Scott; SUBRAMANYAM, Chakrapani; O’DONNELL, Christopher John; AM ENDE, Christopher William; GREEN, Michael Eric; PATEL, Nandini Chaturbhai; STIFF, Cory Michael; TRAN, Tuan Phong; KAUFFMAN, Gregory Wayne; STEPAN, Antonia Friederike; VERHOEST, Patrick Robert; WO2015/49616; (2015); A1;,
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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. 55362-80-6, name is 9-Bromononan-1-ol, molecular formula is C9H19BrO, 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. Recommanded Product: 55362-80-6

A mixture of 9-bromo-1-nonanol (1.1 kg) N, N-dimethylformamide (2.86 L), Imidazole (363 g) Was added to 10 L of the reaction flask, To the ice bath was added dimethyl tert-butylchlorosilane (772 g) Temperature below 20 C, reaction for 1 hour, Add water (5 L), Toluene (1 L), Stir, Dispensing, The aqueous phase was extracted with toluene (1 L) Mixed organic phase, The organic phase was washed with water (1 L) Dried over anhydrous sodium sulfate, At 80 C, Get 1.56 kg product, Directly for the next step reaction

With the rapid development of chemical substances, we look forward to future research findings about 55362-80-6.

Reference:
Patent; Tianjin Pharmaceutical Innovation Co., Ltd.; LIU, WENJUAN; MO, LAN; (14 pag.)CN103965280; (2016); B;,
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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 764-48-7, name is Ethylene Glycol Vinyl Ether. This compound has unique chemical properties. The synthetic route is as follows. category: alcohols-buliding-blocks

In to a reactor, 3.79 parts of the compound represented by formula (I-2-a), 10 parts of tetrahydrofuran and 4.79 parts of triethylamine were charged and stirred at 23 C. for 30 minutes. The obtained mixture was cooled into 0 C. Then, 4.50 parts of the compound represented by formula (I-1-b) was dropped thereto over 30 minutes at 0 C., and the obtained mixture was stirred for 1 hour at 0 C. 100 parts of ethyl acetate, 50 parts of ion exchanged water and 50 parts of a saturated aqueous ammonium chloride solution were added to the resulting reactant, the obtained mixture was stirred at 23 C. for 30 minutes, and left still to separate an organic layer. To the obtained organic layer, 100 parts of ion exchanged water was added, stirred at 23 C. for 30 minutes, and left still, followed by separating an organic layer to wash with water. The washing step was conducted five times. The obtained organic layer was concentrated and purified with column chromatography [silica gel 60N spherical shape, neutral, 100-210 mum, solvent: mixture of n-heptane/ethyl acetate=5/I, manufactured by Kanto Chem. Ltd.], to provide 3.12 parts of the compound represented by formula (I-2-c).

With the rapid development of chemical substances, we look forward to future research findings about 764-48-7.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; NISHIMURA, Takashi; ICHIKAWA, Koji; (98 pag.)US2016/334702; (2016); A1;,
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Electric Literature of 575-03-1, 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. 575-03-1, name is 7-Hydroxy-4-(trifluoromethyl)coumarin, molecular formula is C10H5F3O3, 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.

Commercially available 7-hydroxy-4-trifluoromethyl coumarin (0.069g, 0.30mmol) was dissolved in dry DMF (2.0mL) and then 60percent NaH in mineral oil (0.012g, 0.30mmol) was added while cooling at 0°C. The mixture was slowly warmed at room temperature, then 3-chlorobenzyl bromide (0.040mL, 0.30mmol) was added dropwise via syringe after 1h and stirring was continued for 24h at room temperature. After addition of crushed ice, the suspension was treated with 2.0N aq. solution of NaOH (5mL). The mixture was stirred for 1h and the resulting precipitate was filtered and washed with water, yielding compound 24. White crystals; yield: 84percent, mp: 118.8?120.3°C (ethanol). 1H NMR (300MHz, DMSO-d6) delta: 5.27 (s, 2H), 6.85 (s, 1H), 7.13 (dd, J1=2.4Hz, J2=8.9Hz, 1H), 7.23 (d, J=2.4Hz, 1H), 7.40?7.45 (m, 3H), 7.54 (s, 1H), 7.61?7.64 (m, 1H). Anal. (C17H10ClF3O3) C, H.

According to the analysis of related databases, 575-03-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Pisani, Leonardo; Catto, Marco; Nicolotti, Orazio; Grossi, Giancarlo; Di Braccio, Mario; Soto-Otero, Ramon; Mendez-Alvarez, Estefania; Stefanachi, Angela; Gadaleta, Domenico; Carotti, Angelo; European Journal of Medicinal Chemistry; vol. 70; (2013); p. 723 – 739;,
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Reference of 20605-01-0 ,Some common heterocyclic compound, 20605-01-0, molecular formula is C9H16O6, 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 1 (comparative example) Diethyl 1,5-dioxaspiro[5.5]undecane-3,3-dicarboxylate A stirred mixture of 165.0 g of diethyl bis(hydroxymethyl)malonate (98%, 0.75 mol), 75.3 g of cyclohexanone and 500 g of cyclohexane as a solvent and entrainer was admixed with 1.0 g of sulfuric acid. The mixture was then heated to reflux temperature (70-80 C.), the reaction water formed being continuously removed over a period of 5 hours. After the reaction was complete, the reaction mixture was cooled to room temperature and introduced into dilute, excess aqueous sodium hydrogen carbonate solution. The aqueous phase was re-extracted with methyl t-butyl ether, and the combined organic phases were washed once with water. After drying over sodium sulfate the solvents were distilled off on a rotary evaporator, and the product was isolated by distillation in an oil pump vacuum. This gave 168.4 g of target product (75% of the theoretical yield, based on the diethyl bis(hydroxymethyl)malonate used) with a boiling point of 140 C./0.2 mm. The purity, determined by gas chromatography, was 97 to 98 FID percent by area.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,20605-01-0, its application will become more common.

Reference:
Patent; Huels Aktiengesellschaft; US5932747; (1999); A;,
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