反应详情

温度

100 °C

To 2-chloro-5-(2,3,4,5-tetrahydro-benzo[b]azepine-1-sulfonyl)-phenylamine (3.4 g, 10 mmol) in DCE (20 mL) and HOAc (20 mL) was added urea (1.2 g, 20 mmol). The mixture was stirred at 100° C. for 24 hrs and was then partitioned between DCM (150 mL) and sat. NaHCO3 solution (150 mL). Additional solid NaHCO3 was added until the aqueous layer pH value was 8. The organic layer was separated, washed with saturated NaHCO3 and brine, dried over MgSO4 and evaporated to obtain a yellow oil. The oil was re-dissolved in DCM (10 mL) and ether (50 mL) and stood at rt for 12 hrs to give [2-chloro-5-(2,3,4,5-tetrahydro-benzo[b]azepine-1-sulfonyl)-phenyl]-urea (1.7 g) as a white solid. MS: 379.7 (M+H)+; tR=6.67 min (method 2).

1. customwas then partitioned between DCM (150 mL) and sat. NaHCO3 solution (150 mL)
2. additionAdditional solid NaHCO3 was added until the aqueous layer pH value
3. customThe organic layer was separated
4. washwashed with saturated NaHCO3 and brine
5. dry with materialdried over MgSO4
6. customevaporated
7. customto obtain a yellow oil