1-Bromohexane → HCID 18940413、化合物

HRID 1450187ノート

反応式

HRID 1450187 の反応式
[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

5

反応物 3

HCID 81011-BromohexaneHCID 24758Sodium hydrideHCID 706187411-(Piperazin-1-yl)dibenzo(b,f)(1,4)oxazepine

生成物 1

HCID 18940413HCID 18940413、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

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 rain at room temperature for 20 minutes, and then treated with 1-bromohexane (2.35 g, 12 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 title compound was obtained in 0.167 g (46%) as a light yellow oil.

後処理

  1. stirringThe resulted mixture was stirred at room temperature overnight
  2. customquenched with saturated ammonium chloride solution (10 mL)
  3. extractionThe mixture was extracted with ethyl acetate (3×30 mL)
  4. dry with materialThe combined organic phase was dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated in vacuo to dryness

出典と根拠

ORDレコード
ord-e4c7686493fe4baab4ffe3fef630a837
出典データセット
uspto-grants-1997_02
特許番号
US05602121

反応ノート

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