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Bis(2-Methoxyethyl)amine → HCID 178495933, 화합물

HRID 428417
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HRID 428417 반응식
[CH3:1][O:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][O:8][CH3:9].C[Al](C)C.[Cl:14][C:15]1[CH:35]=[CH:34][C:18]2[C:19](=[O:33])[C:20]3[C:27]([C:28](OCC)=[O:29])=[N:26][NH:25][C:21]=3[C:22](=[O:24])[NH:23][C:17]=2[CH:16]=1>C1(C)C=CC=CC=1>[Cl:14][C:15]1[CH:35]=[CH:34][C:18]2[C:19](=[O:33])[C:20]3[C:27]([C:28](=[O:29])[N:5]([CH2:6][CH2:7][O:8][CH3:9])[CH2:4][CH2:3][O:2][CH3:1])=[N:26][NH:25][C:21]=3[C:22](=[O:24])[NH:23][C:17]=2[CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 2383Bis(2-Methoxyethyl)amineHCID 16682925TrimethylaluminumHCID 1784704817-Chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10-(1H,9H)dione

생성물 1

HCID 178495933HCID 178495933, 화합물수율 330.6%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

Bis-(2-methoxyethyl)amine (560 μL, 3.13 mmol) was added to a solution of trimethylaluminum in toluene (1.56 mL, 3.13 mmol) and the solution was stirred for 20 minutes. A portion (403 μL) of the resulting solution was added to a solution of 7-chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione (100 mg, 0.313 mmol) in toluene (780 μL). The resulting solution was stirred for 24 hours at room temperature and then quenched with an aqueous hydrochloric acid solution (1.8 mL, 1N) and water (15 mL). The aqueous layer was extracted with chloroform (7×25 mL). The organic layers were combined and concentrated on a rotary evaporator. The crude product was purified by flash chromatography eluting with chloroform:2-propanol (99:1-95:5) to give the title compound (421 mg, 67% yield, m.p. 207-209° C.).

후처리

  1. stirringThe resulting solution was stirred for 24 hours at room temperature
  2. customquenched with an aqueous hydrochloric acid solution (1.8 mL, 1N) and water (15 mL)
  3. extractionThe aqueous layer was extracted with chloroform (7×25 mL)
  4. concentrationconcentrated on a rotary evaporator
  5. customThe crude product was purified by flash chromatography
  6. washeluting with chloroform:2-propanol (99:1-95:5)

출처 및 근거

ORD 기록
ord-acc36290687443159eea6eda8608d1bd
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06313290B1

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