HRID1736481

反应详情

EQUATION

反应方程式

HRID 1736481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

38.6 g of the 1-(6-chloropyridin-2-yl)-2-(pyridin-2-yl)ethyl alcohol prepared in the Preparative Example 20, 47.8 g of triphenylphosphine and 26.8 g of phthalimide were dissolved in 500 ml of tetrahydrofuran, followed by the addition thereto of 31.7 g of diethyl azodicarboxylate. The obtained mixture was stirred at room temperature overnight and concentrated, followed by the addition thereto of diethyl ether. The obtained mixture was filtered to remove insolubles and the filtrate was purified by silica gel chromatography (with a hexane/ethyl acetate (2:1) mixture) to give 77.1 g of the title compound as a roughly purified product.

WORKUP

后处理

  1. additionfollowed by the addition
  2. concentrationconcentrated
  3. additionfollowed by the addition
  4. filtrationThe obtained mixture was filtered
  5. customto remove insolubles
  6. customthe filtrate was purified by silica gel chromatography (with a hexane/ethyl acetate (2:1) mixture)