HRID466491

反应详情

EQUATION

反应方程式

HRID 466491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of thionyl chloride (139.0 g, 1.17 mol) in dry DMF (150 ml) was added to a stirred solution of compound 26 (20.0 g, 0.11 mol) in dry DMF (250 ml) at room temperature. The mixture was stirred at room temperature overnight and then poured onto ice-water. The product was extracted into ether (twice), and the combined ethereal extracts were washed with water, saturated sodium hydrogen carbonate, water and dried (MgSO4). The solvent was removed in vacuo to give off-white crystals.

WORKUP

后处理

  1. additionpoured onto ice-water
  2. extractionThe product was extracted into ether (twice), and the combined ethereal extracts
  3. washwere washed with water, saturated sodium hydrogen carbonate, water
  4. dry with materialdried (MgSO4)
  5. customThe solvent was removed in vacuo
  6. customto give off-white crystals