1-Bromohexane → HCID 18940413, 화합물

HRID 1450187노트

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HRID 1450187 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 18940413HCID 18940413, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e4c7686493fe4baab4ffe3fef630a837
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05602121

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