反应 #2345

ord-bc4c5bfd0a2540ebba7d4dbbdd3411b3

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solution was evaporated
  2. 2
    workup.DISSOLUTIONthe residue dissolved in water (15 ml)
  3. 3
    萃取The mixture was extracted three times with dichloromethane
  4. 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%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05728701uspto-grants-1998_03