HRID324917

反应详情

EQUATION

反应方程式

HRID 324917 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The heterogeneous mixture consisting of methylbenzothiazole (59.6 g, 0.4 mol), ortho-phenylenediamine (43.2 g, 0.4 mol) and sulfur (38.4 g, 1.2 mol) in 300 ml of pyridine was heated at the reflux point of pyridine for 22 hours. The reaction mixture was cooled and poured into a solution of brine. After extraction with ethyl acetate, washing of the organic phase 3 times with water, drying over sodium sulfate and concentration of the solvent under vacuum, the solid obtained was washed with acetone. After drying, 2-(1H-benzimidazol-2-yl)benzothiazole (13.8 g, yield: 13%) was obtained in the form of a yellow solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. extractionAfter extraction with ethyl acetate
  3. washwashing of the organic phase 3 times with water
  4. dry with materialdrying over sodium sulfate and concentration of the solvent under vacuum
  5. customthe solid obtained
  6. washwas washed with acetone
  7. customAfter drying