反应详情

温度

40 °C

3-(3-Benzothiazol-6-yl-2-oxo-imidazolidin-1-yl)-isonicotinic acid ethyl ester (I-185a: 0.16 g, 0.4 mmol) in methanolic ammonia (20 mL) was taken in a reaction flask and the flask was heated to 40° C. overnight. The reaction was monitored by TLC (10% MeOH in CHCl3). The reaction mixture was cooled to room temperature and concentrated. The concentrate was partitioned between DCM and water. The organic layer was washed with water, brine, dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (10% MeOH in CHCl3) afforded 40 mg of the product (28.57% yield).

1. temperatureThe reaction mixture was cooled to room temperature
2. concentrationconcentrated
3. customThe concentrate was partitioned between DCM and water
4. washThe organic layer was washed with water, brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. customPurification by column chromatography on silica gel (10% MeOH in CHCl3)