Hydrochloric Acid → Vanillylamine

HRID 968423

반응식

HRID 968423 반응식
Cl.[H][H].Cl.[CH2:5]([NH2:15])[C:6]1[CH:14]=[CH:13][C:11]([OH:12])=[C:8]([O:9][CH3:10])[CH:7]=1>[Pd].O>[CH2:5]([NH2:15])[C:6]1[CH:14]=[CH:13][C:11]([OH:12])=[C:8]([O:9][CH3:10])[CH:7]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 165576Phenol, 4-(aminomethyl)-2-methoxy-, hydrochloride (1:1)HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 70966Vanillylamine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

반응 조건

온도
10 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-7f3ac6f429c74fa8b0b1bdcda7d8dab7
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06958418B2

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