反应详情

温度

-30 °C

In a manner similar to the preparation of compound 2, 12.3 g (0.047 mol) of compound 13 were introduced into a round-bottomed flask which was cooled to -30° C. and had a reflux condenser cooled with dry ice. 5.6 g (0.046 mol) of BCl3 were added to this. When the addition was complete, the cooling bath was removed and the reaction mixture warmed to room temperature and was stirred for 3 hours. The temperature was then raised to 55° C. for 6 hours. After cooling and removal of the volatile contents in vacuo, the crude product was obtained. Distillation under a high vacuum gave the purified product, the main isomer of which was identified as follows:

1. additionwere introduced into a round-bottomed flask which
2. additionWhen the addition
3. customthe cooling bath was removed
4. temperaturethe reaction mixture warmed to room temperature
5. temperatureThe temperature was then raised to 55° C. for 6 hours
6. temperatureAfter cooling
7. customremoval of the volatile contents in vacuo