HRID1750177

反应详情

EQUATION

反应方程式

HRID 1750177 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4.50 g of Boc-L-leucinol in 30 ml of THF were added 4.74 g of p-toluenesulfonylchloride, 7.2 ml of TEA and 0.25 g of DMAP. The reaction was stirred at rt overnight. The pH of the reaction was then adjusted to 6 by the addition of 1 M aqueous hydrochloric acid. The phases were separated and the aqueous phase was extracted with ethyl acetate twice. The combined organic layers were dried over sodium sulphate and concentrated to yield 6.94 g of toluene-4-sulfonic acid (S)-2-tert-butoxycarbonylamino-4-methyl-pentyl ester.

WORKUP

后处理

  1. customThe phases were separated
  2. extractionthe aqueous phase was extracted with ethyl acetate twice
  3. dry with materialThe combined organic layers were dried over sodium sulphate
  4. concentrationconcentrated