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1-Butanol → HCID 71255395, 화합물

HRID 540306
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인쇄 미리보기

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HRID 540306 반응식
Cl[C:2]1[CH:11]=[C:10]([Cl:12])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([Cl:13])[CH:8]=2)[N:3]=1.[Br:14][C:15]1[CH:16]=[CH:17][C:18]2[CH2:24][NH:23][CH2:22][CH2:21][CH2:20][C:19]=2[CH:25]=1.C(O)CCC>C(OCC)(=O)C>[Br:14][C:15]1[CH:16]=[CH:17][C:18]2[CH2:24][N:23]([C:2]3[CH:11]=[C:10]([Cl:12])[C:9]4[C:4](=[CH:5][CH:6]=[C:7]([Cl:13])[CH:8]=4)[N:3]=3)[CH2:22][CH2:21][CH2:20][C:19]=2[CH:25]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 2631-ButanolHCID 187966912,4,6-TrichloroquinolineHCID 533970047-Bromo-2,3,4,5-tetrahydro-1h-benzo[c]azepine

생성물 1

HCID 71255395HCID 71255395, 화합물수율 41%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
160 °C

실험 절차

The mixture of 2,4,6-trichloroquinoline (300 mg, 1.29 mmol), 7-bromo-2,3,4,5-tetrahydro-1H-2-benzazepine (291 mg, 1.29 mmol) and n-butanol (3 mL) was heated with stirring in a 10 mL microwave process vial for 1 hour at 160° C. under microwave irradiation. The mixture was cooled to room temperature and diluted with ethyl acetate (10 mL), and then washed with water (10 mL). The organic layer was dried over sodium sulfate and evaporated to give a residue which was purified by column chromatography on silica gel to give 222 mg of product as a white solid (yield was 41%). MS obsd. (ESI+) [(M+H)+] 421.

후처리

  1. temperaturewas heated
  2. temperatureThe mixture was cooled to room temperature
  3. washwashed with water (10 mL)
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customevaporated
  6. customto give a residue which
  7. customwas purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-bd55cadd7eb14d978f57d74e12359879
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871756B2

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