1,1-Dimethylhydrazine → 5-methoxy-1-tetralone N,N-dimethylhydrazone
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
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
- waitThe mixture was left
- temperatureto cool
- extractionthe mixture was extracted several times with diethyl ether
- dry with materialThe mixture was dried over sodium sulfate
- filtrationfiltered
- customevaporated
- 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
反応ノート
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