HRID1722266

反应详情

EQUATION

反应方程式

HRID 1722266 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.76 g of 4(S,S)-sec.-butyl-2-methyloxazoline and 4.0 ml of N,N,N',N'-tetramethylethylenediamine are dissolved in 100 ml of THF and, at -78° C., added dropwise to 14.9 ml of a 1.6M solution of n-butyllithium in hexane are added dropwise. The mixture is stirred at this temperature for 30 min and then 1.15 g of 3-Boc-4(S)-cyclohexylmethyl-2,2-dimethyl-5(R,S)-iodomethyloxazolidine in 10 ml of THF are added dropwise. The reaction solution is stirred at R.T. for 1 h and is poured into 200 ml of saturated aqueous NaHCO3 solution, and the mixture is extracted 3 times with 200 ml of EA. Drying over Na2SO4 and concentration in vacuo is followed by chromatography on silica gel (mobile phase MTB/diisopropyl ether 1:1). The title compound is obtained as a colorless oil.

WORKUP

后处理

  1. additionare added dropwise
  2. stirringThe reaction solution is stirred at R.T. for 1 h
  3. extractionthe mixture is extracted 3 times with 200 ml of EA
  4. dry with materialDrying over Na2SO4 and concentration in vacuo