HRID1241432
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwere added
- temperatureThe reaction was cooled to room temperature
- filtrationthe precipitate was filtered off
- washwashed with n-butanol and ethyl ether
- customdried
- customto produce 52-3