Ammonium Chloride → 2-Acetylamino-4-aminophenyl beta-hydroxypropyl ether monohydrochloride

HRID 1494288노트

반응식

HRID 1494288 반응식
[Cl-:1].[NH4+].[OH:3][CH:4]([CH3:20])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-])=O)=[CH:9][C:8]=1[NH:16][C:17](=[O:19])[CH3:18]>[Zn]>[ClH:1].[OH:3][CH:4]([CH3:20])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][C:8]=1[NH:16][C:17](=[O:19])[CH3:18]

참가 물질

4

반응물 2

HCID 25517Ammonium ChlorideHCID 198274242-Acetylamino-4-nitrophenyl beta-hydroxypropyl ether

생성물 1

HCID 198274382-Acetylamino-4-aminophenyl beta-hydroxypropyl ether monohydrochloride

시약·촉매·용매 1

HCID 23994Zinc촉매

반응 조건

온도
-20 °C

실험 절차

1.5 g of ammonium chloride and 37.5 g of powdered zinc are added to 70 ml of an aqueous-ethanolic solution (60 ml of C2H5OH/10 ml of H2O) and this mixture is preheated to the reflux temperature, with stirring. 0.048 mol (12.2 g) of 2-acetylamino-4-nitrophenyl β-hydroxypropyl ether is then added, the addition being adjusted so as to maintain the reflux without heating. When the addition has ended, the mixture is kept under reflux for 10 minutes and filtered at the boil onto a mixture of 5 ml of ethanol and 5.1 ml of 36% strength hydrochloric acid, cooled to -20° C. The expected product precipitates in the form of the monohydrochloride. It is filtered off, washed with a small amount of ice-cold ethanol and dried in vacuo at 50° C. It melts with decomposition at between 220° and 225° C.

후처리

  1. additionthe addition
  2. temperatureto maintain the
  3. temperaturereflux
  4. temperaturewithout heating
  5. additionWhen the addition
  6. temperatureunder reflux for 10 minutes
  7. filtrationfiltered at the boil onto a mixture of 5 ml of ethanol and 5.1 ml of 36% strength hydrochloric acid
  8. customThe expected product precipitates in the form of the monohydrochloride
  9. filtrationIt is filtered off
  10. washwashed with a small amount of ice-cold ethanol
  11. customdried in vacuo at 50° C
  12. custommelts with decomposition at between 220° and 225° C.

출처 및 근거

ORD 기록
ord-123eafb5291649339906a64993fb8d32
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05026401

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