HRID1732523

反应详情

EQUATION

反应方程式

HRID 1732523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Partial deprotection of compound XXI (3.4 g, 5.3 mmole) was carried out as described in the previous paragraph. The trifluoroacetate salt (RfC, 0.75) was acylated in DMF (50 ml) with Boc-L-Met-ONp (2.18 g, 5.9 mmole, Bachem) in the presence of DIEA (1.9 ml, 12 mmole) and HOBt (0.9 g, 5.9 mmole). After 4 hr at room temperature the reaction was complete. Evaporation of most of the solvent in vacuo was followed by trituration with EtOAc. The precipitate was washed with EtOAc, with ether and dried: 3.8 g (93%); m.p. 169°-171° C., [α]D24 -21.5° (c 1.2, DMF) RfK, 0.65; RfI, 0.52.

WORKUP

后处理

  1. customEvaporation of most of the solvent in vacuo
  2. washThe precipitate was washed with EtOAc, with ether
  3. customdried