Hydrochloric Acid → Vanillylamine

The reaction mixture obtained in a) is combined with 38 ml of hydrochloric acid and 6.2 g of Pd/C. Hydrogen is piped into the reaction mixture, with stirring, at 10° C. over a period of 4 hours under a pressure of 4 bar. After the addition of 71 ml of water the mixture is heated to 60° C. and stirred for 1 hour. The catalyst is filtered off and the acetic acid is eliminated from the filtrate by distillation at 60° C. Then the reaction mixture is combined with 141 ml of water in order to dissolve the vanillylamine hydrochloride and the salts and stirred at 60° C. for 0.5 hours. After the addition of 99 ml of hydrochloric acid and stirring for 1 hour, the suspension formed is cooled to 3° C. and after 3 hours the vanillylamine hydrochloride is filtered off, washed with acetone and dried at 50° C.

1. customThe reaction mixture obtained in a)
2. temperatureis heated to 60° C.
3. stirringstirred for 1 hour
4. filtrationThe catalyst is filtered off
5. distillationthe acetic acid is eliminated from the filtrate by distillation at 60° C
6. dissolutionto dissolve the vanillylamine hydrochloride
7. stirringthe salts and stirred at 60° C. for 0.5 hours
8. additionAfter the addition of 99 ml of hydrochloric acid
9. stirringstirring for 1 hour
10. customthe suspension formed
11. filtrationis filtered off
12. washwashed with acetone
13. customdried at 50° C.

ORDレコード

ord-7f3ac6f429c74fa8b0b1bdcda7d8dab7

出典データセット

uspto-grants-2005_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06958418B2