Water → N-Acetyl-N-(3-aminophenethyl)amine

HRID 1173126노트

반응식

HRID 1173126 반응식
[C:1]([NH:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-])=O)[CH:8]=1)(=[O:3])[CH3:2].C([O-])(=O)C.[NH4+].O>C(O)C.[Fe]>[C:1]([NH:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([NH2:13])[CH:8]=1)(=[O:3])[CH3:2]

참가 물질

6

반응물 3

HCID 962WaterHCID 517165Ammonium AcetateHCID 22674066N-(3-Nitrophenethyl)acetamide

생성물 1

HCID 22674097N-Acetyl-N-(3-aminophenethyl)amine수율 96%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

N-Acetyl-N-(3-nitrophenethyl)amine (2.1 g, Production Example 28b) was dissolved in ethanol (40 ml). To the mixture were added an iron powder (2.25 g), ammonium acetate (4.3 g) and water (20 ml), followed by heating under reflux for 1.5 hours. Solid was filtered off and washed with ethanol, and then the filtrate was partially evaporated. The residue was extracted with ethyl acetate, washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, to give the title compound (1.723 g, 96%) as a yellow oil.

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 1.5 hours
  3. filtrationSolid was filtered off
  4. washwashed with ethanol
  5. customthe filtrate was partially evaporated
  6. extractionThe residue was extracted with ethyl acetate
  7. washwashed with brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-af677a9849a940ed8aff78446c6cbdf0
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834049B2

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