1,1-Dimethylhydrazine → 5-methoxy-1-tetralone N,N-dimethylhydrazone

HRID 264539

반응식

HRID 264539 반응식
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH2:7][C:8]2=O.[CH3:14][N:15]([CH3:17])[NH2:16]>[Cl-].[Na+]>[CH3:14][N:15]([CH3:17])[N:16]=[C:8]1[C:9]2[C:4](=[C:3]([O:2][CH3:1])[CH:12]=[CH:11][CH:10]=2)[CH2:5][CH2:6][CH2:7]1

참가 물질

4

반응물 2

HCID 59761,1-DimethylhydrazineHCID 366205-Methoxytetralone

생성물 1

HCID 2909415-methoxy-1-tetralone N,N-dimethylhydrazone수율 83%

시약·촉매·용매 1

HCID 5234Sodium Chloride용매

실험 절차

35.25 g of 5-methoxy-1-tetralone and 61 ml of N,N-dimethylhydrazine were heated to about 80° under argon for 5 hours. The mixture was left to cool, 200 ml of 10% sodium chloride solution were added and the mixture was extracted several times with diethyl ether. The mixture was dried over sodium sulfate, filtered and evaporated. The oily residue was distilled over a 10 cm Vigreux column. At 85°-95°/0.1 mbar there were obtained 36.4 g (83%) of 5-methoxy-1-tetralone N,N-dimethylhydrazone as a yellow oil.

후처리

  1. waitThe mixture was left
  2. temperatureto cool
  3. extractionthe mixture was extracted several times with diethyl ether
  4. dry with materialThe mixture was dried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. distillationThe oily residue was distilled over a 10 cm Vigreux column

출처 및 근거

ORD 기록
ord-6b6b4d1f4eac4a8c898806dd0317d33e
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646173

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