反应详情

Method A (free form): A suspension of ethyl 3-{[3-(3-methylquinoxalin-2-yl)-1H-pyrazol-5-yl]amino}-3-oxopropanoate (20.0 g, 58.9 mmol) in 28% aqueous ammonia (295 mL) and methanol (1176 mL) was stirred overnight at room temperature, and then concentrated in vacuo. The residue was diluted with water (1500 mL) and ethyl acetate (1000 mL). The aqueous layer was concentrated in vacuo, and water (40 mL) was added. The mixture was acidified to pH 5-6 with 10% aqueous hydrochloric acid, and then ethanol (360 mL) was added. The resulting precipitate was collected and washed with 95% aqueous ethanol and ethanol to give 2-(3-methylquinoxalin-2-yl)pyrazolo[1,5-a]pyrimidine-5,7-diol. MS (ESI): m/z 292 (M−H).

1. concentrationconcentrated in vacuo
2. additionThe residue was diluted with water (1500 mL) and ethyl acetate (1000 mL)
3. concentrationThe aqueous layer was concentrated in vacuo, and water (40 mL)
4. additionwas added
5. additionethanol (360 mL) was added
6. customThe resulting precipitate was collected
7. washwashed with 95% aqueous ethanol and ethanol