反应详情

温度

0 °C

A mixture of Step 2 intermediate (8.0 g, 47.01 mmol) and acetic anhydride (40 ml) in dry pyridine (78 ml) were refluxed for 3 h. The reaction mixture was cooled to 0° C. and acidified with 1N HCl (200 ml). The solid obtained was collected by filtration, washed with 1 N HCl (25 ml), water (25 ml) and dried to give 6.9 g of the product as a white solid; 1H NMR (300 MHz, DMSO-d6): δ 2.71 (s, 3H), 2.96 (s, 3H), 3.37 (s, 3H), 3.50 (s, 3H).

1. customThe solid obtained
2. filtrationwas collected by filtration
3. washwashed with 1 N HCl (25 ml), water (25 ml)
4. customdried