HRID435478

反应详情

EQUATION

反应方程式

HRID 435478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.95 g (0.025 moles) of D,L-carnitine hydrochloride are dissolved in 8 mls of CF3COOH, and to the solution an excess (16 mls) of p-isobutylphenyl-alpha-methyl acetyl chloride is added and the mixture is kept under stirring at a temperature of 40°-45° C. for 4-5 hours. At the end of this period of time, the mixture is partitioned with H2O--CHCl3, the organic phase is discarded whereas the aqueous phase is concentrated under reduced pressure at a bath temperature of about 50° C. A gelatinous raw material is obtained which is crystallized with isopropanol. The precipitate thus obtained is filtered, rapidly washed with ether because of its hydroscopicity, and dried under vacuum at a temperature not exceeding 50° C.; 6.3 g of a product are obtained (yield 65%) having the following characteristics:

WORKUP

后处理

  1. customAt the end of this period of time, the mixture is partitioned with H2O--CHCl3
  2. concentrationis concentrated under reduced pressure at a bath temperature of about 50° C
  3. customA gelatinous raw material is obtained which
  4. customis crystallized with isopropanol
  5. customThe precipitate thus obtained
  6. filtrationis filtered
  7. washrapidly washed with ether because of its hydroscopicity
  8. customdried under vacuum at a temperature not
  9. customexceeding 50° C.