HRID2231285

反应详情

EQUATION

反应方程式

HRID 2231285 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A stirred mixture of 2-hydroxybenzo(b)thiophene-3-carboxamide (0.485 g, 0.0025 m), diphenylacetaldehyde (0.51 g, 0.0026 m), p. toluenesulfonic acid hydrate (30 mg), and dried toluene (15 ml) is set in an oil-bath at 100° C., the bath temperature raised to 150° C., and the mixture heated under reflux until thin-layer chromatography of the mixture indicates completeness of reaction. The cooled reaction mixture is concentrated in vacuo and the residue chromatographed on silica gel (v/v 10-50% CH2Cl2 in hexane) to yield N-(2,2-Diphenylethenyl)-2-hydroxybenzo(b)thiophene-3-carboxamide.

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureunder reflux until thin-layer chromatography of the mixture
  3. customcompleteness of reaction
  4. customThe cooled reaction mixture
  5. concentrationis concentrated in vacuo
  6. customthe residue chromatographed on silica gel (v/v 10-50% CH2Cl2 in hexane)