HRID1164699

反应详情

EQUATION

反应方程式

HRID 1164699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

p-Hydrazino benzoic acid (152 mg, 1 mmol) and bis-(p-methoxyphenyl)-telluroxide (394 mg, 1.10 mmol) were stirred in chloroform (10 ml) at room temperature for 24 h. The reaction mixture was then poured into saturated aqueous potassium carbonate, the phases separated and the aqueous phase extracted with dichloromethane (2×10 ml). The combined organic phases were dried over sodium sulphate and evaporated under reduced pressure. The residue after purification by column chromatography (chloroform) gave bis-(p-methoxyphenyl)-telluride (151 mg, 44%). The aqueous phase, on acidification with hydrochloric acid and extraction with dichloromethane gave a yellow solid (54 mg) which on sublimation under reduced pressure gave pure benzoic acid (32 mg, 26%) m.p. 122° (lit., 122°).

WORKUP

后处理

  1. customthe phases separated
  2. extractionthe aqueous phase extracted with dichloromethane (2×10 ml)
  3. dry with materialThe combined organic phases were dried over sodium sulphate
  4. customevaporated under reduced pressure
  5. customThe residue after purification by column chromatography (chloroform)