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HCID 57565297, 화합물 → HCID 57565299, 화합물

HRID 1727053
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HRID 1727053 반응식
[F:1][C:2]([F:31])([F:30])[C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([S:15]([C:18]3[CH:19]=[C:20]4[C:24](=[CH:25][CH:26]=3)[N:23](C(=O)C)[CH2:22][CH2:21]4)(=[O:17])=[O:16])[CH2:11][CH2:10]2)=[CH:5][CH:4]=1>O1CCOCC1>[F:30][C:2]([F:1])([F:31])[C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:10][CH2:11][N:12]([S:15]([C:18]3[CH:19]=[C:20]4[C:24](=[CH:25][CH:26]=3)[NH:23][CH2:22][CH2:21]4)(=[O:16])=[O:17])[CH2:13][CH2:14]2)=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 57565297HCID 57565297, 화합물

생성물 1

HCID 57565299HCID 57565299, 화합물수율 75%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

1-{5-[4-(4-Trifluoromethyl-phenyl)-piperazine-1-sulfonyl]-2,3-dihydro-indol-1-yl}-ethanone was refluxed in 1,4-dioxane (5 mL) and concentrate HCl (2.5 mL) for 2 h. The reaction was then diluted with dichloromethane and washed with 1N HCl, saturated sodium bicarbonate, dried (Na2SO4), filtered and concentrated to provide 5-[4-(4-trifluoromethyl-phenyl)-piperazine-1-sulfonyl]-2,3-dihydro-1H-indole (1.03 g, 75%) as an off-white solid. 1H NMR (400 MHz, CDCl3) 7.48-7.20 (m, 4H), 6.88 (d, 2H), 6.60 (d, 1H), 3.70 (t, 2H), 3.36-3.33 (m, 4H), 3.15-3.12 (m, 4H), 3.10 (t, 2H).

후처리

  1. concentrationconcentrate HCl (2.5 mL) for 2 h
  • additionThe reaction was then diluted with dichloromethane
  • washwashed with 1N HCl, saturated sodium bicarbonate
  • dry with materialdried (Na2SO4)
  • filtrationfiltered
  • concentrationconcentrated
  • 출처 및 근거

    ORD 기록
    ord-244bd2c99e514d5b84d519de25d41abe
    출처 데이터셋
    uspto-grants-2009_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07494999B2

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