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

HRID 1494288ノート

反応式

HRID 1494288 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 23994Zinc触媒

反応条件

温度
-20 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-123eafb5291649339906a64993fb8d32
出典データセット
uspto-grants-1991_06
特許番号
US05026401

反応ノート

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