HRID858300

反应详情

EQUATION

反应方程式

HRID 858300 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.5 g of 1-acetyl-6-chloro-2-indolinone, 3.4 g of 1-methylbenzimidazole-5-carboxylic acid, 6.1 g of TBTU, 2.9 g of HOBT-hydrate and 8.7 ml ethyldiisopropylamine are stirred in 100 ml DMF for 15 hours at ambient temperature. The mixture is combined with water and extracted with ethyl acetate, while the crude product is partially precipitated. The residue obtained by distilling off the solvent is taken up in dichloromethane and a little methanol and extracted with water. The organic phase is evaporated down, the residue stirred successively with ethyl acetate and diethyl ether, suction filtered and dried.

WORKUP

后处理

  1. extractionextracted with ethyl acetate, while the crude product
  2. customis partially precipitated
  3. customThe residue obtained
  4. distillationby distilling off the solvent
  5. extractiona little methanol and extracted with water
  6. customThe organic phase is evaporated down
  7. filtrationfiltered
  8. customdried