HRID1081932

反应详情

EQUATION

反应方程式

HRID 1081932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

37.2 g of 5-iodo vanillin (commercial) and 360 ml of dichloromethane were mixed together under nitrogen and the mixture was cooled to 0° C. 135 ml of a molar solution of boron tribromide in dichloromethane were added and the mixture stood for 16 hours at ambient temperature and was then concentrated, cooled to 0° C. and acidified. The crystallized product was separated out, washed with water, dried and crystallized from an isopropanol-water mixture (1-2 by volume) to obtain 23.4 g of the expected product.

WORKUP

后处理

  1. concentrationwas then concentrated
  2. temperaturecooled to 0° C.
  3. customThe crystallized product was separated out
  4. washwashed with water
  5. customdried
  6. customcrystallized from an isopropanol-water mixture (1-2 by volume)