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Dipropylamine → HCID 178457279, 화합물

HRID 1954732
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HRID 1954732 반응식
C[Al](C)C.[CH2:5]([NH:8][CH2:9][CH2:10][CH3:11])[CH2:6][CH3:7].[Cl:12][C:13]1[CH:33]=[CH:32][C:16]2[C:17](=[O:31])[C:18]3[C:25]([C:26]([O:28]CC)=O)=[N:24][NH:23][C:19]=3[C:20](=[O:22])[NH:21][C:15]=2[CH:14]=1>C1(C)C=CC=CC=1>[Cl:12][C:13]1[CH:33]=[CH:32][C:16]2[C:17](=[O:31])[C:18]3[C:25]([C:26](=[O:28])[N:8]([CH2:9][CH2:10][CH3:11])[CH2:5][CH2:6][CH3:7])=[N:24][NH:23][C:19]=3[C:20](=[O:22])[NH:21][C:15]=2[CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

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HCID 8902DipropylamineHCID 16682925TrimethylaluminumHCID 1784704817-Chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10-(1H,9H)dione

생성물 1

HCID 178457279HCID 178457279, 화합물수율 31%

시약·촉매·용매 1

HCID 1140Toluene용매3회

실험 절차

To a solution of trimethylaluminum in toluene (4.68 mL 9.38 mmol) was added dipropylamine (1.29 mL, 9.38 mmol) and the solution was stirred for 45 hours. A portion (1.9 30 mL) of this solution was added to a solution of 7-chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione (500 mg, 1.56 mmol) in toluene (2 mL). Additional toluene (7 mL) was added. The solution was stirred for 70 minutes at room temperature and then quenched with 1N hydrochloric acid (9.3 mL). The layers were separated and the aqueous layer was extracted with ethyl acetate (3×50 mL). The combined organics were washed with 1N hydrochloric acid and water (25 mL) and concentrated by rotary evaporation. The crude residue was purified by chromatography eluting with hexanes:ethyl acetate (95:5-50:50) to give the title compound (31% yield, m.p. 270° C.).

후처리

  1. stirringThe solution was stirred for 70 minutes at room temperature
  2. customquenched with 1N hydrochloric acid (9.3 mL)
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with ethyl acetate (3×50 mL)
  5. washThe combined organics were washed with 1N hydrochloric acid and water (25 mL)
  6. concentrationconcentrated by rotary evaporation
  7. customThe crude residue was purified by chromatography
  8. washeluting with hexanes:ethyl acetate (95:5-50:50)

출처 및 근거

ORD 기록
ord-6ad9b8fea0924976b03a40b1b1b3bf2e
출처 데이터셋
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06124281

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