HRID1732522

反应详情

EQUATION

反应方程式

HRID 1732522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The Boc group was removed from a sample (3.8 g, 6.6 mmole) of compound XX as described above. The partially deprotected 2-peptide ester (trifluoroacetate salt) was dissolved in DMF (60 ml) and treated with DIEA (2.4 ml, 15 mmole), HOBt (1.18 g, 7.7 mmole) and Boc-L-Ala-ONp (2.38 g, 7.7 mmole, Bachem) at 0°. After overnight storage at room temperature a semisolid mass formed. Most of the solvent was removed in vacuo, the residue triturated with EtOAc and with ether and dried: 3.6 g (85%), m.p. 140°-143° C.; [α]D23 -21.8° (c 0.8 DMF); RfB, 0.85; RfI, 0.62.

WORKUP

后处理

  1. customAfter overnight storage at room temperature a semisolid mass formed
  2. customMost of the solvent was removed in vacuo
  3. customthe residue triturated with EtOAc and with ether
  4. customdried