HRID6795
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
PROCEDURE
实验过程
The product (208 mg, 1.0 mmol) from Step B and piperidine (0.5 mL, 5 mmol) were mixed in absolute ethanol (3 mL) and then heated at reflux for 4 h. The reaction mixture was cooled to r.t., and the solvent removed under vacuum. The solids were taken up in EtOAc (125 mL). The mixture was transferred to a separatory funnel and washed with water (3×15 mL). The organic layer was dried over sodium sulfate, filtered and the solvent removed under vacuum to afford the product as a yellow solid, MS: m/z 258 (MH+) which was used without further purification.
WORKUP
后处理
- temperatureheated
- temperatureat reflux for 4 h
- customthe solvent removed under vacuum
- customThe mixture was transferred to a separatory funnel
- washwashed with water (3×15 mL)
- dry with materialThe organic layer was dried over sodium sulfate
- filtrationfiltered
- customthe solvent removed under vacuum