HRID1600082

反应详情

EQUATION

反应方程式

HRID 1600082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

0.3 g of 2-{[1-(4-chloro-1-naphthyl)-5-(2,6-dimethoxyphenyl)-3-pyrazolyl]carbonylamino}hexanoic acid is dissolved in 6.7 ml of dichloromethane and the mixtureis cooled to -70° C. 5.7 ml of boron tribromide, dissolved in 20 ml of dichlormethane, are added dropwise and the reaction mixture is left for2 hours at -70° C. It is allowed to return to room temperature, and 12 ml of water are then added while cooling. Concentrated NaOH is added topH 14. The aqueous phase is washed with ether and brought to pH 2, the product is extracted with ethyl acetate and the organic phase is dried over sodium sulphate, filtered and evaporated. The residue is crystallisedfrom diisopropyl ether.

WORKUP

后处理

  1. additionare added dropwise
  2. waitthe reaction mixture is left for2 hours at -70° C
  3. customto return to room temperature
  4. temperaturewhile cooling
  5. washThe aqueous phase is washed with ether
  6. extractionthe product is extracted with ethyl acetate
  7. dry with materialthe organic phase is dried over sodium sulphate
  8. filtrationfiltered
  9. customevaporated