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Sodium Carbonate → HCID 178449972, 화합물

HRID 1433180
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HRID 1433180 반응식
[C:1]([NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[CH:25]=[CH:24][C:18]2[NH:19][C:20]([CH2:22]Cl)=[N:21][C:17]=2[CH:16]=1)(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2].[F:26][C:27]([F:36])([F:35])[C:28]1[CH:29]=[CH:30][C:31]([OH:34])=[CH:32][CH:33]=1.C([O-])([O-])=O.[Na+].[Na+].C([O-])([O-])=O.[Cs+].[Cs+]>CC(C)=O>[C:1]([NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[CH:25]=[CH:24][C:18]2[NH:19][C:20]([CH2:22][O:34][C:31]3[CH:30]=[CH:29][C:28]([C:27]([F:26])([F:35])[F:36])=[CH:33][CH:32]=3)=[N:21][C:17]=2[CH:16]=1)(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 10340Sodium CarbonateHCID 10796Cesium carbonateHCID 678744-(Trifluoromethyl)phenolHCID 178449971HCID 178449971, 화합물

생성물 1

HCID 178449972HCID 178449972, 화합물수율 30.6%

시약·촉매·용매 1

HCID 180Acetone
용매

실험 절차

A mixture of N-tert-butyl-2-(2-chloromethyl-1H-benzoimidazol-5-yl)benzenesulfonamide (100 mg, 0.26 mmol), α,α,α-trifluoro-p-cresol (43.0 mg, 0.26 mmol), Na2CO3 (28.1 mg, 0.26 mmol), Cs2CO3 (86.5 mg, 0.26 mmol), and catalytic KI (1.5 mg, 0.009 mmol) in acetone (2 mL) was refluxed for 12 h. The reaction mixture was concentrated under reduced pressure, and the residue was purified by chromatography (silica, EtOAc: hexanes, 1:1) to afford the title compound as an off-white solid (40.1 mg, 30% yield). Calcd. For C25H24F3N3O3S: 504.54 (M+H), Found 504.2.

후처리

  1. temperaturewas refluxed for 12 h
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customthe residue was purified by chromatography (silica, EtOAc: hexanes, 1:1)

출처 및 근거

ORD 기록
ord-ac4398f35721440c8b4a62709c4f140c
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612211B2

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