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
N-[2-Cyano-3-(1,4-dihydro-1-phenyl-indeno[1,2-c]pyrazol-3-yl) -3-oxo-propanoyl]-glycine, methyl ester (1.7 g), is suspended in 1% KOH solution in 95% ethanol (60 ml) and heated under stirring at the reflux temperature for 30 minutes. After cooling the precipitate is filtered and washed with ethanol, then dissolved in water. The aqueous basic solution is extracted with ethyl acetate and then acidified to pH 3 with 2N HCl. The precipitate is extracted with ethyl acetate and the organic solution washed with N HCl and then with water until neutral. Evaporation to dryness in vacuo gives a residue which is crumbled with ethanol to yield 1.2 g of N-[2-cyano-3-(1,4-dihydro 1-phenyl-indeno[1,2-c]pyrazol-3-yl)-3-oxo-propanoyl]-glycine, m.p. 247°-249° C. dec.
WORKUP
后处理
- temperatureheated
- temperatureAfter cooling the precipitate
- filtrationis filtered
- washwashed with ethanol
- dissolutiondissolved in water
- extractionThe aqueous basic solution is extracted with ethyl acetate
- extractionThe precipitate is extracted with ethyl acetate
- washthe organic solution washed with N HCl
- customEvaporation to dryness in vacuo
- customgives a residue which