L-VALINE, N-[(2'-CYANO[1,1'-BIPHENYL]-4-YL)METHYL]-, METHYL ESTER, MONOHYDROCHLORIDE synthesis
- Product Name:L-VALINE, N-[(2'-CYANO[1,1'-BIPHENYL]-4-YL)METHYL]-, METHYL ESTER, MONOHYDROCHLORIDE
- CAS Number:482577-59-3
- Molecular formula:C20H23ClN2O2
- Molecular Weight:358.86
6306-52-1
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$5.00/5g
114772-54-2
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482577-59-3
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$27.00/5g
Yield:482577-59-3 260 g
Reaction Conditions:
with potassium carbonate in water;ethyl acetate for 2 h;Reflux;
Steps:
2 Preparation of secondary amine methyl ester hydrochloride:
800 ml of drinking water and 240 g of potassium carbonate were charged into the reactor,Stirring into the 2000ml ethyl acetate,168 g of L-valine methyl ester hydrochloride prepared in Example 1 and 200 g of bromo-sarbazine.Heated to reflux and maintained reflux for 2 hours.Cold to 20 ~ 40 after standing, sub-water,The organic phase was acidified with hydrochloric acid to pH = 1. Filtration at 70 ± 5 ° C,Vacuum degree of -0.09Mpa under the drying, the secondary amine methyl ester hydrochloride 260g, purity 99.6%.
References:
Tsingtao Xuejie Zhuji Co., Ltd.;Chen Likun;Liu Linxue;Li Jianmin CN103923028, 2017, B Location in patent:Paragraph 0055-0056