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Acetaldehyde → 1-(3,4-Methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride

HRID 26001
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HRID 26001 반응식
[ClH:1].[CH2:2]1[O:10][C:9]2[CH:8]=[CH:7][C:6]([CH:11]([OH:14])[CH2:12][NH2:13])=[CH:5][C:4]=2[O:3]1.[CH:15](=O)[CH3:16].[H][H]>[Ni].C(O)C>[ClH:1].[CH2:2]1[O:10][C:9]2[CH:8]=[CH:7][C:6]([CH:11]([OH:14])[CH2:12][NH:13][CH2:15][CH3:16])=[CH:5][C:4]=2[O:3]1
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참가 물질

6

반응물 3

HCID 177AcetaldehydeHCID 14318106HCID 14318106, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 213260981-(3,4-Methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

18 g. of 1-(3,4-methylenedioxyphenyl)-2-aminoethanol hydrochloride are dissolved in 300 ml. of ethanol and 50 ml. of 80% aqueous solution of acetaldehyde. To the resulting solution are added 0.5 g. of extended Raney nickel and the mixture is heated at 70° C. in an atmosphere of hydrogen in a 1 liter-autoclave. After the absorption of hydrogen is complete, the mixture is cooled. Then the catalyst is filtered off and the filtrate is concentrated to dryness. Upon recrystallization of the crude crystalline residue from isopropyl alcohol, 12.5 g. of 1-(3,4-methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride are obtained as white needles.

후처리

  1. additionTo the resulting solution are added 0.5 g
  2. customAfter the absorption of hydrogen
  3. temperaturethe mixture is cooled
  4. filtrationThen the catalyst is filtered off
  5. concentrationthe filtrate is concentrated to dryness
  6. customUpon recrystallization of the crude crystalline residue from isopropyl alcohol, 12.5 g

출처 및 근거

ORD 기록
ord-551580bfd33349668c8de1563891ed34
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04147799

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