HRID82500

反应详情

EQUATION

反应方程式

HRID 82500 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-(Hydroxymethyl)benzoic hydrazide CAS [58855-42-8] (1.4 g, 8.4 mmol) in ethanol (14 mL) were added carbon disulfide (1.12 mL, 18.5 mmol) and triethyl amine (1.3 mL, 9.3 mmol). After heating to reflux for 16 h with stirring, the reaction mixture was diluted with ethyl acetate. The mixture was washed with 10% HCl solution and brine, dried over magnesium sulfate, and concentrated. Purification of the residue by MPLC (65% ethyl acetate in hexanes) gave 1.62 g of [4-(5-Mercapto-1,3,4-oxadiazol-2-yl)phenyl]methanol as a colorless solid.

WORKUP

后处理

  1. temperatureAfter heating
  2. temperatureto reflux for 16 h
  3. washThe mixture was washed with 10% HCl solution and brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customPurification of the residue by MPLC (65% ethyl acetate in hexanes)