HRID1743201
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of 1′-benzyl-3-(4-isopropylphenyl)-4,6,7-trimethylspiro[benzofuran-2(3H),4′-piperidine]-5-ol (3.51 g, 7.70 mmol) and triethylamine (1.1 mL, 7.9 mmol) in chloroform (40 mL) α-chloroethyl chloroformate (2.30 g, 16.1 mmol) was added at 0° C. The mixture was refluxed for 1 hour and concentrated under reduced pressure. The residue was refluxed in methanol (20 mL) for 1 hour and concentrated under reduced pressure. The residue was crystallized from ethanol-ethyl acetate to obtain the title compound (2.80 g, yield 90%).
WORKUP
后处理
- temperatureThe mixture was refluxed for 1 hour
- concentrationconcentrated under reduced pressure
- temperatureThe residue was refluxed in methanol (20 mL) for 1 hour
- concentrationconcentrated under reduced pressure
- customThe residue was crystallized from ethanol-ethyl acetate