HRID2383826
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
NaH (32.8 mg, 1.3705 mmol) and DMF (4 mL) was added to 1-[3-fluoro-4-(1-hydroxyimino-ethyl)-phenyl]-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one (111b: 150 mg, 0.4568 mmol). The resulting mixture was microwaved at 50° C. for 1 hour. The reaction was monitored by TLC (10% MeOH in DCM). The reaction mixture was partitioned between ice water and ethylacetate. The organic layer was washed with water, brine solution, dried over Na2SO4 and concentrated under reduced pressure. Purification by column chromatography on silica gel (5% MeOH in CHCl3) afforded 15 mg of the product (10.7% yield).
WORKUP
后处理
- customThe resulting mixture was microwaved at 50° C. for 1 hour
- customThe reaction mixture was partitioned between ice water and ethylacetate
- washThe organic layer was washed with water, brine solution
- dry with materialdried over Na2SO4
- concentrationconcentrated under reduced pressure
- customPurification by column chromatography on silica gel (5% MeOH in CHCl3)