Water → 2-(3,4-Dimethoxyphenyl)-N-ethylethan-1-amine

HRID 2253611

반응식

HRID 2253611 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([NH:10][CH2:11][CH2:12][C:13]1[CH:22]=[CH:21][C:18]([O:19][CH3:20])=[C:15]([O:16][CH3:17])[CH:14]=1)(=O)[CH3:8].O>O1CCCC1.C(OCC)(=O)C>[CH2:7]([NH:10][CH2:11][CH2:12][C:13]1[CH:22]=[CH:21][C:18]([O:19][CH3:20])=[C:15]([O:16][CH3:17])[CH:14]=1)[CH3:8]

참가 물질

6

반응물 3

HCID 962WaterHCID 80465N-Acetyl-3,4-dimethoxyphenethylamineHCID 21226445Aluminium lithium hydride

생성물 1

HCID 107509132-(3,4-Dimethoxyphenyl)-N-ethylethan-1-amine

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매3회HCID 8857Ethyl Acetate용매

실험 절차

To a suspension of 0.98 g of lithium aluminum hydride in 50 ml of dried tetrahydrofuran (THF), a solution of 3 g of N-acetylhomoveratrylamin in 25 ml of THF was added dropwise with stirring. After heating for 3 hours under reflux, the reaction mixture was cooled with ice and gradually added dropwise under violent stirring with a solvent mixture composed of 10 ml of water and 10 ml of THF. Insoluble matter was filtered off and the filtrate was concentrated. The residue obtained was dissolved in 50 ml of ethyl acetate, washed twice with water and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, N-ethyl-homoveratrylamine was obtained as oily product. The yield was 2.3 g.

후처리

  1. temperatureAfter heating for 3 hours
  2. temperatureunder reflux
  3. temperaturethe reaction mixture was cooled with ice
  4. additiongradually added dropwise
  5. stirringunder violent stirring with a solvent mixture
  6. filtrationInsoluble matter was filtered off
  7. concentrationthe filtrate was concentrated
  8. customThe residue obtained
  9. washwashed twice with water
  10. dry with materialdried over anhydrous sodium sulfate
  11. distillationAfter distilling off the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-c9507609662b4f75a45498dac1674a81
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05232923

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