反应详情

温度

120 °C

2-Fluoro-5-[3-(4-methyl-pyridin-3-yl)-2-oxo-imidazolidin-1-yl]-benzoic acid methyl ester (I-117a: 510 mg, 1.55 mmol) and hydrazine hydrate were taken in a reaction flask and the flask was heated to 120° C. for 18 hours with stirring. The reaction was monitored by TLC (10% MeOH in CHCl3). The reaction mixture was partitioned between ice water and ethylacetate. The aqueous layer was concentrated to afford the solid residue which was dissolved in 1:1 DCM: MeOH and filtered. The filtrate was concentrated and purified by column chromatography on silica gel (10-15% MeOH in CHCl3). The residue was washed with DCM and dried to afford 180 mg of the product (37.6% yield).

1. customThe reaction mixture was partitioned between ice water and ethylacetate
2. concentrationThe aqueous layer was concentrated
3. customto afford the solid residue which
4. filtrationMeOH and filtered
5. concentrationThe filtrate was concentrated
6. custompurified by column chromatography on silica gel (10-15% MeOH in CHCl3)
7. washThe residue was washed with DCM
8. customdried