反应详情

温度

80 °C

Prop-2-en-1-yl 7-(3,4-diaminophenyl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (2.7 g, 7.96 mmol) was taken into glacial acetic acid (15 mL) followed by addition of 1,3-(dimethoxycarbonyl)-2-methyl-2-thiopseudourea (1.81 g, 8.8 mmol) and the mixture was heated to 80° C. for 30 minutes then concentrated to a thick residue. The residue was treated with saturated aqueous sodium bicarbonate and the aqueous mixture basified with portionwise addition of solid sodium bicarbonate with pH 8-9. The aqueous mixture was then partitioned with hexanes then filtered. The filter cake was washed with water then hexanes and dried to give prop-2-en-1-yl 7-(2-{[(methyloxy)carbonyl]amino}-1H-benzimidazol-5-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (3.46 g, 100% yield) as a pale yellow solid.

1. concentrationthen concentrated to a thick residue
2. additionThe residue was treated with saturated aqueous sodium bicarbonate
3. additionthe aqueous mixture basified with portionwise addition of solid sodium bicarbonate with pH 8-9
4. customThe aqueous mixture was then partitioned with hexanes
5. filtrationthen filtered
6. washThe filter cake was washed with water
7. dry with materialhexanes and dried