HRID84592

反应详情

EQUATION

反应方程式

HRID 84592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 8-bromo-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-2-carboxylic acid (396 mg) in dry dichloromethane (20 mL) was added oxalyl chloride (180 μL) and DMF (1 drop). After 3 hours the solvent was removed in vacuo and to the residue was added acetonitrile (20 mL), 2-chloroaniline (140 μL) and sodium bicarbonate (111 mg). After 3 hours, water was added to the reaction mixture and the resulting precipitate was collected by filtration to yield 8-bromo-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-2-carboxylic acid (2-chloro-phenyl)-amide (467 mg).

WORKUP

后处理

  1. customAfter 3 hours the solvent was removed in vacuo and to the residue
  2. additionwas added acetonitrile (20 mL), 2-chloroaniline (140 μL) and sodium bicarbonate (111 mg)
  3. additionwater was added to the reaction mixture
  4. filtrationthe resulting precipitate was collected by filtration