HRID2308612

反应详情

EQUATION

反应方程式

HRID 2308612 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.6 g (0.01 mol) of 4-chloro-2-trifluoromethylbenzenesulfonamide were dissolved in 20 ml of pyridine, 2-chloroisonicotinoyl chloride was added dropwise at room temperature. Agitation was then continued for 2 hr. at the same temperature. The reaction mixture was acidified by adding aqueous hydrochloric acid, and the precipitate thus formed was extracted by ethyl acetate. The organic layer obtained was dried and then concentrated to precipitate crude crystals, which were recrystallized by solvent mixture of n-hexane and ethyl acetate to produce 3.4 g (yield: 85.1%) of N-(4-chloro-2-trifluoromethylphenylsulfonyl)-2-chloroisonicotinamide as white crystals.

WORKUP

后处理

  1. customthe precipitate thus formed
  2. extractionwas extracted by ethyl acetate
  3. customThe organic layer obtained
  4. customwas dried
  5. concentrationconcentrated
  6. customto precipitate crude crystals, which
  7. customwere recrystallized by solvent mixture of n-hexane and ethyl acetate