HRID82500
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter heating
- temperatureto reflux for 16 h
- washThe mixture was washed with 10% HCl solution and brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customPurification of the residue by MPLC (65% ethyl acetate in hexanes)