HRID1943304

反应详情

EQUATION

反应方程式

HRID 1943304 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 5.39 g of H-Lys(Boc)-OtBu hydrochloride (15.9 mmol, 1.0 eq) and 7.1 ml of triethylamine (50.9 mmol, 3.2 eq) in dichloromethane (70 ml) was added to the solution obtained in Example 143d), in such a way that the temperatures did not exceed 10° C. After the addition was complete, the mixture was allowed to reach RT and was stirred for a further 2 h. The reaction mixture was then mixed with 200 ml of 0.2 M hydrochloride acid, and the organic phase was separated off and washed with 100 ml of 0.2 M hydrochloric acid and concentrated. 5.5 g of the desired material were obtained as a colorless oil, which crystallized on standing.

WORKUP

后处理

  1. customdid not exceed 10° C
  2. additionAfter the addition
  3. customto reach RT
  4. customthe organic phase was separated off
  5. washwashed with 100 ml of 0.2 M hydrochloric acid
  6. concentrationconcentrated