反应 #2345
ord-bc4c5bfd0a2540ebba7d4dbbdd3411b3
反应方程式
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他The solution was evaporated
- 2workup.DISSOLUTIONthe residue dissolved in water (15 ml)
- 3萃取The mixture was extracted three times with dichloromethane
- 4其他Evaporation of the combined extracts
实验过程
The compound of Example 140 (0.96 g) in TFA (10 ml) was kept at room temperature for 2 hours. The solution was evaporated and the residue dissolved in water (15 ml) and the solution basified with sodium carbonate. The mixture was extracted three times with dichloromethane. Evaporation of the combined extracts gave the title compound (0.56 g); m.p. 125°-127° C.; NMR(d6DMSO) δ 8.2(2H,d), 6.92(6H,m), 4.0(2H,m), 3.64(3H,s), 3.46(4H,t), 3.15(4H,t), 2.04(2H,m), 1.84(1H, m); m/e 371(M+H)+. Calculated for C20H26N4 O3. 0.75 H2O: C, 62.5; H, 7.17; N, 14.6. Found: C, 62.8; H, 6.8; N, 14.3%.