反应详情

温度

75 °C

To 4.6 L of water at room temperature in a 4-neck 50 L flask sitting in a steam bath apparatus equipped with an overhead stirrer, a temperature probe and reflux condenser was added 3.72 Kg (27.36 mol) of sodium acetate with stirring, followed by 1.9 Kg of hydroxylamine hydrochloride (27.36 mol). To this slurry at room temperature, 12 L of ethanol was added followed by 1.994 Kg (13.68 mol) of 1-tetralone. Additional ethanol (1.7 L) was used to rinse off the funnel and added to the reaction mixture. The resulting light orange slurry was heated to 75° C. over 40 minutes and maintained at 75°-85° C. for another 75 minutes. The reaction mixture was cooled with the aid of ice packed around the flask. When the internal temperature reached 32° C., the reaction mixture was pumped over 15 minutes into 60 L of ice contained in a 200 L vessel. The reaction vessel was washed with an additional 2 L of water which was added to the 200 L vessel. When the ice melted, the mixture was filtered through a filter pad and the wet cake washed with 4 L of water. The wet cake was suction dried for 1 hour then transferred to two trays and dried under vacuum at 40° C. for 2 days to give 2.094 Kg (13.01 mol, 95%) of product. 1H NMR (250 MHz,CDCl3): 1.90 (m,2H), 2.80 (t,6 Hz,2H), 2.88 (t,6 Hz,2H), 7.15-7.35 (m,3H), 7.90 (d,8 Hz,1H), 8.9 (br s,1H).

1. customapparatus equipped with an overhead stirrer
2. temperaturea temperature probe and reflux condenser
3. washto rinse off the funnel
4. additionadded to the reaction mixture
5. temperaturemaintained at 75°-85° C. for another 75 minutes
6. temperatureThe reaction mixture was cooled with the aid of ice
7. customreached 32° C.
8. customcontained in a 200 L vessel
9. washThe reaction vessel was washed with an additional 2 L of water which
10. additionwas added to the 200 L vessel
11. filtrationthe mixture was filtered through a filter pad
12. washthe wet cake washed with 4 L of water
13. customdried for 1 hour
14. customdried under vacuum at 40° C. for 2 days