反应详情

温度

0 °C

22.13 g (100 mmol) of the product obtained in Step 1, suspended in 250 mL of THF, are cooled to 0° C. There are then added, dropwise, over 15 minutes, 250 mL of borane/THF (1M in the THF) and heating is carried out at 80° C. for 24 hours. Cooling is carried out and there are then added, dropwise, 250 mL of ethanol, and then 2.6N ethanolic HCl. Heating at reflux is carried out for 40 minutes; some light insoluble material is filtered off and evaporation to dryness is carried out. The residue thereby obtained is recrystallised from a mixture of 150 mL of isopropanol and 20 mL of water to yield the desired product.

1. additionThere are then added
2. waitis carried out at 80° C. for 24 hours
3. temperatureCooling
4. additionthere are then added
5. temperatureHeating
6. temperatureat reflux
7. waitis carried out for 40 minutes
8. filtrationsome light insoluble material is filtered off
9. customevaporation to dryness
10. customThe residue thereby obtained
11. customis recrystallised from a mixture of 150 mL of isopropanol and 20 mL of water