HRID963088

反应详情

EQUATION

反应方程式

HRID 963088 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(4-(3-(2-Chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazol-3-ylmethyl)indole-2-carboxamide (1.0 g, Example 14) was dissolved in acetic acid (12 ml). Bromine (0.1 ml) dissolved in acetic acid (1 ml) was dropwise added under water-cooling, and the mixture was stirred for 1 hour. The solvent was evaporated, and an aqueous sodium thiosulfate solution was added. The mixture was extracted with chloroform. The extract was washed with saturated brine, a saturated aqueous sodium hydrogencarbonate solution and saturated brine, and dried over magnesium sulfate. The solvent was evaporated, and the residue was recrystallized from methanol to give 0.36 g of N-(4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazol-3-ylmethyl)-3-bromoindole-2-carboxamide.

WORKUP

后处理

  1. additionwas dropwise added under water-
  2. temperaturecooling
  3. customThe solvent was evaporated
  4. additionan aqueous sodium thiosulfate solution was added
  5. extractionThe mixture was extracted with chloroform
  6. washThe extract was washed with saturated brine
  7. dry with materiala saturated aqueous sodium hydrogencarbonate solution and saturated brine, and dried over magnesium sulfate
  8. customThe solvent was evaporated
  9. customthe residue was recrystallized from methanol