反应详情

温度

40 °C

To a reaction vessel, 3,4-diethoxy-2-fluoro-6-formylbenzonitrile (5.90 kg, 24.87 mol) and ethyl acetate (59.0 L) were added under a nitrogen atmosphere, followed by addition of sodium triacetoxyborohydride (NaB(OAc)3H) (11.70 kg) while stirring. After stirring for 30 min, the inside temperature was raised to 40° C., and the reaction solution was stirred for 2 hours. Then, the reaction solution was cooled. Water (2 L) was added thereto slowly and dropwise at the inside temperature of 15° C. to thereby decompose excessive sodium triacetoxyborohydride. Water (27.5 L) was further added thereto. The temperature of the external bath was raised to 40° C. to dissolve insoluble matter, followed by re-cooling and separation of liquid layers. The resultant organic layer was washed with aqueous sodium bicarbonate solution twice and then with saline. The thus obtained organic layer was cooled with the external bath temperature of 10° C. and left overnight.

1. stirringAfter stirring for 30 min
2. stirringthe reaction solution was stirred for 2 hours
3. temperatureThen, the reaction solution was cooled
4. customdropwise at the inside temperature of 15° C.
5. temperatureThe temperature of the external bath was raised to 40° C.
6. dissolutionto dissolve insoluble matter
7. temperatureby re-cooling
8. customseparation of liquid layers
9. washThe resultant organic layer was washed with aqueous sodium bicarbonate solution twice
10. temperatureThe thus obtained organic layer was cooled with the external bath temperature of 10° C.