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

HRID 264539

反応式

HRID 264539 の反応式
[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

参加物

4

反応物 2

HCID 59761,1-DimethylhydrazineHCID 366205-Methoxytetralone

生成物 1

HCID 2909415-methoxy-1-tetralone N,N-dimethylhydrazone収率 83%

試薬・触媒・溶媒 1

HCID 5234Sodium Chloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6b6b4d1f4eac4a8c898806dd0317d33e
出典データセット
uspto-grants-1997_07
特許番号
US05646173

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