反应详情

温度

115 °C

6.88 g (30 mmol) of N-(1-cyanocyclopentyl)pentanamide (content 84.7 percent), 16.66 g of dried butanol and 10.06 g (39 mmol) of a freshly-prepared 14.13 percent solution of hydrogen chloride in butanol were heated to the reflux point (preheated oil bath) under nitrogen, with stirring, and product precipitated out as soon as the internal temperature reached ca. 100° C. After 2.9 hours of reflux (115° C.), the mixture was cooled to 1° C. and left to stand for 1 hour at this temperature. The product which had precipitated out was filtered off, washed with 10 ml of ice-cold butanol and dried at 40° C./24 mbar. The yield of the product was 4.93 g (66 percent), content 92.7 percent (HPLC).

1. customproduct precipitated out as soon as the internal temperature
2. customreached ca. 100° C
3. temperaturethe mixture was cooled to 1° C.
4. waitleft
5. customThe product which had precipitated out
6. filtrationwas filtered off
7. washwashed with 10 ml of ice-cold butanol
8. customdried at 40° C./24 mbar