Aniline → Benzenamine, N-(2-methylcyclohexyl)-
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][C:10]1=O.N1C2C=CC=CC=2N=N1.[BH4-].[Na+]>O.CO>[CH3:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH:10]1[NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
7
実験手順
In a 100-mL flask, the following mixture is heated at reflux for 30 h: 9.3 g aniline, 11.2 g 2-methylcyclohexanone and 12 g benzotriazole. Then, 200 mL of methanol and 5 g of NaBH4 in portions are added to the mixture, which is then heated at reflux for 30 min. The solution is allowed to cool, and 100 mL of water are added to the mixture, which is extracted with 2×100 mL diisopropyl ether. The organic phase is recovered, dried over magnesium sulfate and reduced to dryness. In this manner, 7 g of the desired amine are produced.
後処理
- temperatureIn a 100-mL flask, the following mixture is heated
- temperatureat reflux for 30 h
- temperatureis then heated
- temperatureat reflux for 30 min
- temperatureto cool
- extractionis extracted with 2×100 mL diisopropyl ether
- customThe organic phase is recovered
- dry with materialdried over magnesium sulfate
出典と根拠
- ORDレコード
- ord-61e704a2dd6541a4a35c55c83857e054
- 出典データセット
- uspto-grants-1999_12
- 特許番号
- US06004486
反応ノート
読み込み中…