反应详情

温度

40 °C

2-{[(Benzyloxy)carbonyl]amino}-2-methylpropanoic acid (5.18 g, 21.83 mmol) in a mixture of pyridine (25 mL) and DMF (25 mL) was treated with 1,1′-carbonyldiimidazole (3.72 g, 22.92 mmol) and heated at 40° C. for 2 hours. 2,3-Diaminobenzamide dihydrochlolide (4.89 g, 21.83 mmol), prepared as described in WO0026192, was added and the mixture was stirred at room temperature overnight. The solvents were removed under vacuum and the residue was partitioned between ethyl acetate and diluted sodium bicarbonate aqueous solution. The formed slightly yellow solid material was collected by filtration, washed with water and ethyl acetate, and dried to give Example 1A. MS (DCI/NH3) m/z 371 (M+H)+.

1. additionwas added
2. customThe solvents were removed under vacuum
3. customthe residue was partitioned between ethyl acetate and diluted sodium bicarbonate aqueous solution
4. customThe formed slightly yellow solid material
5. filtrationwas collected by filtration
6. washwashed with water and ethyl acetate
7. customdried
8. customto give Example 1A