HRID2383805
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
1-(3-Acetyl-4-fluoro-phenyl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one (160 mg, 0.513 mmol) in hydrazine hydrate (5 mL) was taken in a reaction flask and the flask was heated to reflux and maintained for 21 hours. The reaction was monitored by TLC (10% MeOH in CHCl3). The reaction mixture was partitioned between ethylacetate and water. The organic layer was dried over Na2SO4, filtered and the filtrate was concentrated. Purification by column chromatography on silica gel (3% MeOH in CHCl3), followed by preparative HPLC afforded 22 mg of the product (14% yield).
WORKUP
后处理
- temperaturethe flask was heated
- temperatureto reflux
- temperaturemaintained for 21 hours
- customThe reaction mixture was partitioned between ethylacetate and water
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationthe filtrate was concentrated
- customPurification by column chromatography on silica gel (3% MeOH in CHCl3)