Month: May 2021

Synthetic Route of 13330-96-6, 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.13330-96-6, name is 4-(Dimethylamino)butan-1-ol, molecular formula is C6H15NO, molecular weight is 117.19, as common compound, the synthetic route is as follows.

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.

Statistics shows that 13330-96-6 is playing an increasingly important role. we look forward to future research findings about 4-(Dimethylamino)butan-1-ol.

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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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. 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol. A new synthetic method of this compound is introduced below., Safety of 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol

To a solution of the perfluoroalkyl alcohol (10 mmol) in 10 mLof dry THF, was added sodium hydride (60% 1.4 equiv. dissolved in 2 mL of dry THF in oil) at 0 C under nitrogen atmosphere. The mixture was stirred for 30 min. Then 1.35 g (10 mmol) of henylisothiocyanate was added. The reaction mixture was allowed to warm to room temperature and stirred for 3 h. The mixture was quenched with saturated aqueous ammonium chloride. The aqueous layer was washed with diethyl ether and the combined organic layers were dried over Na2SO4. The solvent was removed by vacuum evaporation and the crude products were purified with column chromatography on silica gel (70-230 meshes) using petroleum ether/diethyl ether (8:2) as eluent or recrystallized in cyclohexane to give the corresponding O-perfluoroalkyl thiocarbamate.

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, 647-42-7, 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol.

Reference:
Article; Chniti, Ines; Sanhoury; Chehidi; Journal of Fluorine Chemistry; vol. 156; (2013); p. 101 – 105;,
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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. 19819-98-8, name is 2-(o-Tolyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows. SDS of cas: 19819-98-8

To a stirred solution of tert-butyl 4-([(5-chloro-2-hydroxybenzoyl)amino]methyl}benzoate (step 1 of the synthetic procedure of example 1-4, 0.21 g, 0.58 mmol), 2-(2-methylphenyl)ethanol (0.16 g, 1.2 mmol) and triphenylphosphine (0.30 g, 1.2 mmol) in tetrahydrofuran (5 mL) was added di-tert-butyl azodicarboxylate (0.27 g, 1.2 mmol) at room temperature. After being stirred overnight, the reaction was quenched by the addition of sodium bicarbonate aqueous solution. The aqueous layer was extracted with ethyl acetate and the combined organic layers were washed with brine, dried (magnesium sulfate), and evaporated. The remaining residue was purified by flush column chromatography on silica gel eluding with hexane/ethyl acetate (5/1) to afford 0.21 g (76%) of the title compounds as a colorless oil: 1H-NMR (CDCl3) 8.20 (1H, d, J=2.8 Hz), 7.99 (1H, t, J=5.9 Hz), 7.91 (2H, d, J=8.2 Hz), 7.38 (1H, dd, J=8.7, 2.8 Hz), 7.25 (2H, d, J=8.2 Hz), 7.16-7.03 (4H, m), 6.93 (1H, d, J=8.7 Hz), 4.52 (2H, d, J=5.9 Hz), 4.34 (2H, t, J=6.8 Hz), 3.04 (2H, t, J=6.8 Hz), 2.25 (3H, s), 1.59 (9H, s); MS (ESI) m/z 480 (M+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, 19819-98-8, 2-(o-Tolyl)ethanol.

Reference:
Patent; Pfizer Inc; US2005/250818; (2005); A1;,
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Reference of 3637-61-4 ,Some common heterocyclic compound, 3637-61-4, 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.

The toluene 4-sulfonic acid cyclopentyl methyl ester was prepared by adding p- Toluenesulfonyl chloride (3.6 mmol, 684 mg) to a solution of CYCLOPENTANEMETHANOL (3 mmol, 300mg) and pyridine (3ml) in dichloromethane (3ml). The resulting mixture was stirred for 2 1/2 hours at room temperature, then diluted with DICHLOROMETHANE and washed sequentially with HCI (1 M solution) and a saturated solution of NA2CO3. The organic layer was then dried over MgSO4 and evaporated to give the TOLUENE-4-SULFONIC acid cyclopentyl methyl ester.1H NMR (CDCI3) delta 1.17 (2H, m), 1.53 (4H, m), 1.69 (2H, m), 2.20 (1H, m), 2.45 (3H, s), 3.89 (2H, d), 7.34 (2H, d), 7.78 (2H, d).

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. 3637-61-4, Cyclopentanemethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXO GROUP LIMITED; WO2004/39753; (2004); A2;,
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Reference of 57772-50-6, 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.57772-50-6, name is (2-Amino-3-methylphenyl)methanol, molecular formula is C8H11NO, molecular weight is 137.18, as common compound, the synthetic route is as follows.

EXAMPLE 13 2-Amino-3-methylbenzyl alcohol (1.7 g.) and anhydrous chloral (2.4 ml.) were mixed for 10 minutes with external ice-cooling, and the mixture was left to stand for 1/2 hour. The mixture was then chromatographed on silica, and elution with diethyl ether/petroleum ether (b.p. 60-80 C.), 7:3 by volume, gave 1,2-dihydro-8-methyl-2-trichloromethyl-4H-benzo[d]-[1,3]-oxazine, which was crystallized from aqueous ethanol, m.p. 69-70 C. The process described above was repeated, using the appropriate o-aminobenzyl alcohol as starting material, to give the following analogous products:

The chemical industry reduces the impact on the environment during synthesis 57772-50-6, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Imperial Chemical Industries Limited; US4268510; (1981); A;,
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Adding a certain compound to certain chemical reactions, such as: 55414-72-7, (2-Amino-5-methoxyphenyl)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, 55414-72-7, blongs to alcohols-buliding-blocks compound. Recommanded Product: 55414-72-7

In a 50 mL round bottom flask, 2 mmol of 2-amino-5-methoxybenzyl alcohol (Formula (1-3)), 2 mmol of benzaldehyde (Formula (2-1)), 0.2 mmol of ABNO, 0.6 was added. The KOH of mmol and the toluene of 4mL replace the air in the bottle with oxygen, seal the bottle mouth with a rubber stopper and insert an oxygen balloon.The reaction flask was placed in a pre-heated oil bath and heated to 80C for 5 hours.The solvent was distilled off under reduced pressure and then subjected to column chromatography. The mixture of ethyl acetate/petroleum ether having a volume ratio of 1:50 was used as an eluent to collect the eluent containing the target compound, and the solvent was distilled off to obtain the product 6- Methoxy-2-phenyl-4H-3,1-benzoxazine with isolated yield of 94%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,55414-72-7, its application will become more common.

Reference:
Patent; Zhejiang University of Technology; Shen Zhenlu; Li Meichao; Ma Jiaqi; Hu Xinquan; Hu Baoxiang; (13 pag.)CN106831632; (2017); A;,
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Related Products of 7735-42-4, Adding some certain compound to certain chemical reactions, such as: 7735-42-4, name is 1,16-Hexadecanediol,molecular formula is C16H34O2, 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 7735-42-4.

4.2 1 6-Bromohexadecan- 1 -ol10215] The diol 14 (1.047 g, 4.05 mmol) was dissolved in cyclohexane (30 mE) and vigorously stirred with 48% HBr (0.5 mE, 4.46 mmol, 1.1 eq.). The mixture was refluxed for 6 h, diluted with water (50 mE) and the phases were separated. The aqueous phase was extracted with a mixture of dichloromethane and methanol (v/v, 4:1 3×20 mE). The combined organic layer was dried over Mg504. The product was purified by column chromatography with silica gel (6×6 cm, cyclohexane/ethyl acetate, 8:1) and isolated as a white solid. Yield: 4.598 g (96%). Traces of i,i6-dibromohexadecane were also found.1515 13 11 9 7 5 3 1j0216] M.p.: 65 C. (lit. 53-54 C.)j0217] ?H-NMR (300 MHz, CDC13) oe [ppm]: 1.26-1.47 (m, 23H, 4-CH2 to i4-CH2, i-OH), 1.51-1.62 (m, 4H, 2-CH2, 3-CH2), 1.85 (m, 2H, i5-CH2), 3.41 (t, 3JH,H=6.9 Hz, 2H, i6-CH2), 3.64 (t, 3J,y=6.6 Hz, 2H, i-CH2).10218] ?3C-NMR (75 MHz, CDC13) oe [ppm]: 25.9 (t, C-3),28.3, 28.9, 29.6, 29.7, 29.8 (t, C-4 to C-i4), 33.0 (t, C-2, C-iS), 34.3 (t, C-i6), 63.3 (t, C-i).10219] Refs.: M.p. P. Chuit, J. Hausser, Helv. Chim. Acta1929, 12, 850-859.10220] ?H-NMR spectroscopic data agree with those given by: S. Takanashi, M. Takagi, H. Takikawa; K. Mori, I Chem. Soc., Perkin Trans. 11998, 1603-1606.

According to the analysis of related databases, 7735-42-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; WESTFAELISCHE WILHELMS-UNIVERSITAET MUENSTER; Haufe, Guenter; Levkau, Bodo; Schaefers, Michael; Schilson, Stefani Silke; Keul, Petra; US2014/170067; (2014); A1;,
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Related Products of 37585-25-4, 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. 37585-25-4, name is (2-Amino-5-chlorophenyl)methanol, molecular formula is C7H8ClNO, 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: Benzyl alcohol derivative 11 (1 eq.) was dissolved in CH2Cl2 (0.4 M). Manganese (IV) oxide (2.1 eq.)was added under argon and the solution was left to stir at room temperature for 48 h. The progress ofthe reaction was monitored by TLC analysis. After completion, manganese oxide was filtered off andthe resulting filtrate was concentrated under reduced pressure. The crude product was purified by silicacolumn chromatography employing mixtures of n-hexane and ethyl acetate as eluents to obtain thedesired product 10.

According to the analysis of related databases, 37585-25-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Jarrige, Lucie; Merad, Jeremy; Zaied, Siwar; Blanchard, Florent; Masson, Geraldine; Synlett; vol. 28; 14; (2017); p. 1724 – 1728;,
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Reference of 22348-44-3, 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.22348-44-3, name is trans-4-(Methylamino)cyclohexanol, molecular formula is C7H15NO, molecular weight is 129.2, as common compound, the synthetic route is as follows.

EXAMPLE 161 2-Acetamino-5-bromo-4-tert.butyl-N-(trans-4′-hydroxy-cyclohexyl)-N-methyl-benzylamine, m.p. 174-176 C, was prepared from 2-acetamino-5-bromo-4-tert.butyl-benzyl bromide and trans-4-methylamino-cyclohexanol analogous to Example 4.

Statistics shows that 22348-44-3 is playing an increasingly important role. we look forward to future research findings about trans-4-(Methylamino)cyclohexanol.

Reference:
Patent; Boehringer Ingelheim GmbH; US4101671; (1978); A;,
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Related Products of 7218-43-1, 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 7218-43-1 as follows.

Weigh 200mg of 1-adamantanacetic acid, dissolve it in 3mL of dichloromethane, add DCC, DMAP successively under ice bath, stir for 30min under ice bath, add 156mg of intermediate 6, The reaction was performed at room temperature for 5 hours. After the reaction was detected to be complete by LC-MS, the insoluble matter was removed by filtration, and dichloromethane (20 mL x 3) was added. Extracted twice with 20 mL of saturated sodium bicarbonate, dried by adding anhydrous MgSO4 for 5 h, filtered with suction, and purified by column chromatography under reduced pressure to obtain 180 mg of intermediate H-1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,7218-43-1, its application will become more common.

Reference:
Patent; Zhengzhou University; Ke Yu; Xie Hang; Liu Hongmin; Xu Xia; Liang Jianjia; (25 pag.)CN110759897; (2020); A;,
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