HRID863272

反应详情

EQUATION

反应方程式

HRID 863272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.52 g of the ethyl 9-benzyloxy-5(S)-tert-butoxycarbonylamino-4(R,S)-hydroxy-7,7-dimethyl-nonanoate obtained as the crude product are refluxed in 100 ml of toluene and 4 ml of glacial acetic acid at 110° C. under argon for 4.5 h. After the reaction mixture has cooled, it is diluted with ethyl acetate and worked up in the customary manner. The crude product is purified by chromatography over silica gel (mobile phase B), the two 5(S) and 5(R) stereoisomers being separated. This gives the pure title compound (diastereomer I) as a yellowish oil: Rf (B)=0.26; FAB-MS: (M+H)+ =406; and diastereomer II: Rf (B)=0.22.

WORKUP

后处理

  1. temperatureAfter the reaction mixture has cooled
  2. customThe crude product is purified by chromatography over silica gel (mobile phase B)
  3. customthe two 5(S) and 5(R) stereoisomers being separated