HRID1241432

反应详情

EQUATION

反应方程式

HRID 1241432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

N-isopropyl-2-piperazin-1-ylacetamide 13-1 (0.74 g, 4.0 mmol)) was suspended in n-butanol to which compound 52-2 (0.85 g, 4.0 mmol) and triethylamine (1.22 g, 12.0 mmol) were added and then heated at 150° C. for 6 hours. The reaction was cooled to room temperature and the precipitate was filtered off, washed with n-butanol and ethyl ether and dried to produce 52-3. Rf=0.45 (DCM:MeOH:NH4OH, 95:5:0.5). 1H-NMR (DMSO-d6): 11.16(s, 1H); 8.33(s, 1H); 7.54(d, 1H); 7.36(s, 1H); 7.05(s, 1H); 6.24(s, 1H); 3.90(m, 1H); 3.55(br s, 4H); 2.94(s, 2H); 2.49(br s, 4H); 1.08(d, 6H).

WORKUP

后处理

  1. additionwere added
  2. temperatureThe reaction was cooled to room temperature
  3. filtrationthe precipitate was filtered off
  4. washwashed with n-butanol and ethyl ether
  5. customdried
  6. customto produce 52-3