HRID54811

反应详情

EQUATION

反应方程式

HRID 54811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 0° C. solution of 14.67 g of product from Example 274 in 200 ml of 3:1 diethyl ether/water is treated with 4.99 g of sodium bicarbonate and 15.07 g of iodine. The reaction minute is stirred vigorously for 24 hours at room temperature, quenched with 15 ml of saturated sodium sulfite, and diluted with 100 ml of water. the reaction minute is extracted with diethyl ether, dried, concentrated in vacuo, and purified by chromatography (silica gel: 0-10% ethyl acetate/hexane) to give 15.0 g of the desired product.

WORKUP

后处理

  1. customquenched with 15 ml of saturated sodium sulfite
  2. additiondiluted with 100 ml of water
  3. extractionthe reaction minute is extracted with diethyl ether
  4. customdried
  5. concentrationconcentrated in vacuo
  6. custompurified by chromatography (silica gel: 0-10% ethyl acetate/hexane)