HRID1642336
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of 3-(2-Nitro-benzoylamino)-1H-furo[3,2-c]pyrazole-5-carboxylic acid (1-methyl-1-phenyl-ethyl)-amide (1 g, 0.0023 mol) in ethanol (30 mL) tin chloride dihydrate (2.08 g, 0.00923 mol) was added. The mixture was heated to reflux for 4 hours. After cooling, the solvent was evaporated to dryness and the crude purified by flash column chromatography on silica gel (eluting with dichloromethane-methanol 4713. The isolated product was triturated with ethyl ether and dry under vacuum, furnishing 550 mg of the title compound (59% yield).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 4 hours
- temperatureAfter cooling
- customthe solvent was evaporated to dryness
- customthe crude purified by flash column chromatography on silica gel (
- washeluting with dichloromethane-methanol 4713
- customThe isolated product was triturated with ethyl ether
- customdry under vacuum