Dimethylethylamine → N-(4-Ethoxy-3-methoxy-phenethyl)-ethylenediamine

HRID 2121589노트

반응식

HRID 2121589 반응식
[NH2:1][CH2:2][CH2:3][NH:4][C:5](=O)[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH3:15])=[C:9]([O:16][CH3:17])[CH:8]=1.[AlH3].N(CC)(C)C>C1COCC1>[CH2:14]([O:13][C:10]1[CH:11]=[CH:12][C:7]([CH2:6][CH2:5][NH:4][CH2:3][CH2:2][NH2:1])=[CH:8][C:9]=1[O:16][CH3:17])[CH3:15]

참가 물질

5

반응물 3

HCID 11723DimethylethylamineHCID 14488Aluminum hydrideHCID 22034123N-(2-amino-ethyl)-2-(4-ethoxy-3-methoxy-phenyl)acetamide

생성물 1

HCID 22034119N-(4-Ethoxy-3-methoxy-phenethyl)-ethylenediamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Treat a solution of N-(2-amino-ethyl)-2-(4-ethoxy-3-methoxy-phenyl)acetamide (0.7 g, 2.77 mmol) in THF (10 mL) with AlH3.NMe2Et (55 mL, 27.74 mmol) and heat to reflux for 14 h. Cool the resulting mixture to ambient temperature, quench with Na2CO3.10H2O (0.5 g) and stir at ambient temperature for 15 min. Filter the solution through Celite and wash with several portions of CH2Cl2. Concentrate the filtrate in vacuo and purify by preparative TLC (10% MeOH in CH2Cl2) to obtain the title compound as a white oil.

후처리

  1. temperatureto reflux for 14 h
  2. customquench with Na2CO3.10H2O (0.5 g)
  3. filtrationFilter the solution through Celite
  4. washwash with several portions of CH2Cl2
  5. concentrationConcentrate the filtrate in vacuo
  6. custompurify by preparative TLC (10% MeOH in CH2Cl2)

출처 및 근거

ORD 기록
ord-f1b4a94bd23446f3b64585effab5c354
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06696445B2

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