反应详情

To a solution of 1′-benzyl-3-(4-isopropylphenyl)-4,6,7-trimethylspiro[benzofuran-2(3H),4′-piperidine] (10.26 g, 23.34 mmol) in tetrahydrofuran (100 ml) was added α-chloroethyl chloroformate (3.76 g, 26.60 mmol) and the resulting mixture was refluxed with heating for 1 hour. The reaction mixture was cooled down to room temperature and concentrated under reduced pressure. Methanol (80 ml) was added into the resulting residue and the mixture was refluxed for 1 hour. The reaction mixture was cooled down to room temperature and concentrated under reduced pressure. The residue was crystallized from ethanol to obtain 7.32 g (81% yield) of the title compound. Melting point: >260° C. (decomposed).

1. temperaturethe resulting mixture was refluxed
2. temperaturewith heating for 1 hour
3. concentrationconcentrated under reduced pressure
4. additionMethanol (80 ml) was added into the resulting residue
5. temperaturethe mixture was refluxed for 1 hour
6. temperatureThe reaction mixture was cooled down to room temperature
7. concentrationconcentrated under reduced pressure
8. customThe residue was crystallized from ethanol