反应详情

According to Scheme 9 Step 1: A mixture of N-(3-(4-(4-chlorobenzyl)-6-methoxy-3,5-dioxo-4,5-dihydro-1,2,4-triazin-2(3H) yl)phenyl)acetamide (500 mg, 1.24 mmol) in a solution 6N of HCl (10 mL) and THF (10 mL) was stirred at reflux for 3 hours. The THF was evaporated and the aqueous layer was basified with saturated solution of NaHCO3 until neutral pH. The aqueous layer was then extracted with ethyl acetate (×3). The organic layers were combined to be successively washed with water then with brine, dried over MgSO4, filtered and concentrated. The crude product was azeotroped with acetonitrile to afford 2-(3-aminophenyl)-4-(4-chlorobenzyl)-6-methoxy-1,2,4-triazine-3,5(2H,4H)-dione as a beige solid (423 mg, 94.5%).

1. temperatureat reflux for 3 hours
2. customThe THF was evaporated
3. extractionThe aqueous layer was then extracted with ethyl acetate (×3)
4. washto be successively washed with water
5. dry with materialwith brine, dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude product was azeotroped with acetonitrile