HRID2294912
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A stirred solution of 0.52 g of trans-1,3-dihydro-1-{4-[4-(tert-butyloxycarbonyl)piperazin-1-yl]-1-cyclohexyl}-2H-benzimidazol-2-one in 15 mL of 1N HCl was heated to reflux for 1 h, cooled, basified to pH 10 with 6N NaOH and extracted 2×50 mL of CHCl3. The combined extracts were dried over MgSO4 and concentrated under reduced pressure. After drying overnight under vacuum, there was obtained 0.28 g of trans-1,3-dihydro-1-{4-(1-piperazinyl)-1-cyclohexyl}-2H-benzimidazol-2-one as a white solid: 1H NMR (400 MHz, CDCl3) 7.14 (m, 1H), 7.11 (m, 1H), 7.07 (m, 2H), 4.28 (m, 1H), 2.61 (s, 4H), 2.45 (t, 1H), 2.26 (q, 2H), 2.10 (d, J=12.2, 2H), 2.0 (d, J=10.8, 2H), 1.53 (q, 2H).
WORKUP
后处理
- temperatureto reflux for 1 h
- temperaturecooled
- extractionextracted 2×50 mL of CHCl3
- dry with materialThe combined extracts were dried over MgSO4
- concentrationconcentrated under reduced pressure
- customAfter drying overnight under vacuum