1-Bromohexane → HCID 18940413、化合物
反応式
[N:1]1([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[O:11][C:10]3[CH:18]=[CH:19][CH:20]=[CH:21][C:9]=3[N:8]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[H-].[Na+].Br[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30]>CN(C=O)C>[CH2:25]([N:4]1[CH2:3][CH2:2][N:1]([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[O:11][C:10]3[CH:18]=[CH:19][CH:20]=[CH:21][C:9]=3[N:8]=2)[CH2:6][CH2:5]1)[CH2:26][CH2:27][CH2:28][CH2:29][CH3:30]参加物
反応条件
- 温度
- 0 °C
実験手順
To a stirred solution of 11-(1-piperazinyl)dibenz[b,f][1,4]oxazepine (0.28 g, 1.00 mmol) in DMF (10 mL) was added sodium hydride (0.056 g, 60% in oil, 1.40 mmol) at 0° C. under argon. The mixture was stirred at 0° C. for 10 min at room temperature for 20 minutes, and then treated with 1 -bromohexane (0.198 g, 1.2 mmol). The resulted mixture was stirred at room temperature overnight and quenched with saturated ammonium chloride solution (10 mL). The mixture was extracted with ethyl acetate (3×30 mL). The combined organic phase was dried over magnesium sulfate and filtered. The filtrate was concentrated in vacuo to dryness and the residue was subjected to column chromatography using ethyl acetate/hexane (1/2) as the eluent. The desired compound, 11-(4-hexyl-1-piperazinyl)dibenz[b,f][1,4]oxazepine, was obtained in 0.167 g (46%) as a light yellow oil.
後処理
- stirringThe resulted mixture was stirred at room temperature overnight
- customquenched with saturated ammonium chloride solution (10 mL)
- extractionThe mixture was extracted with ethyl acetate (3×30 mL)
- dry with materialThe combined organic phase was dried over magnesium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo to dryness
出典と根拠
- ORDレコード
- ord-36da358ebcf4470db1be73088f438815
- 出典データセット
- uspto-grants-1998_11
- 特許番号
- US05834459
反応ノート
読み込み中…