HRID490886

反应详情

EQUATION

反应方程式

HRID 490886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of Intermediate 19 (0.045 g) in THF (2 ml) was treated with DIPEA (0.045 ml), then with cyclopropylcarbonyl chloride (0.013 g) and stirred at room temperature for 16 h. The mixture was concentrated in vacuo and the residue partitioned between dichloromethane and water. The layers were separated and the organic layer concentrated in vacuo, then applied to an SPE cartridge (aminopropyl, 1 g). The column was eluted with methanol to afford Intermediate 20 as a white solid (0.02 g). LCMS showed MH+=373; TRET=2.15 min.

WORKUP

后处理

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue partitioned between dichloromethane and water
  3. customThe layers were separated
  4. concentrationthe organic layer concentrated in vacuo
  5. washThe column was eluted with methanol