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Potassium Carbonate → HCID 86702226, 화합물

HRID 83834
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HRID 83834 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([S:35](O)(=[O:37])=[O:36])[CH:5]=[C:6]([F:34])[C:7]=1[CH2:8][S:9][C:10]1[N:11]([C:27]2[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=2)[C:12]([C:15]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[C:20]([O:25][CH3:26])[CH:19]=2)([CH3:17])[CH3:16])=[CH:13][N:14]=1.S(Cl)(Cl)=O.Cl.[Cl-].[NH2:45][CH2:46][CH2:47][C:48]1[CH:49]=[N+:50]([CH3:54])[CH:51]=[CH:52][CH:53]=1.C([O-])([O-])=O.[K+].[K+]>C(Cl)Cl.CC#N.CN(C=O)C>[Cl-:1].[Cl:1][C:2]1[CH:3]=[C:4]([S:35]([NH:45][CH2:46][CH2:47][C:48]2[CH:49]=[N+:50]([CH3:54])[CH:51]=[CH:52][CH:53]=2)(=[O:36])=[O:37])[CH:5]=[C:6]([F:34])[C:7]=1[CH2:8][S:9][C:10]1[N:11]([C:27]2[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=2)[C:12]([C:15]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[C:20]([O:25][CH3:26])[CH:19]=2)([CH3:16])[CH3:17])=[CH:13][N:14]=1
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HCID 11430Potassium CarbonateHCID 24386Thionyl ChlorideHCID 67234778HCID 67234778, 화합물HCID 867022273-chloro-5-fluoro-4-((5-(2-(4-fluoro-3-methoxyphenyl)propan-2-yl)-1-(4-fluorophenyl)-1H-imidazol-2-ylthio)methyl)benzenesulfonic acid

생성물 1

HCID 86702226HCID 86702226, 화합물수율 11.3%

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

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온도
50 °C

실험 절차

To a suspension of 3-chloro-5-fluoro-4-((5-(2-(4-fluoro-3-methoxyphenyl)propan-2-yl)-1-(4-fluorophenyl)-1H-imidazol-2-ylthio)methyl)benzenesulfonic acid (250 mg, 0.43 mmol) in DCM (5 mL) was added thionyl chloride (1 mL) and DMF (10 uL, anhyd). The reaction mixture was heated 2 h at 50° C., concentrated, diluted with DCM, and concentrated to dryness. The sulfonyl chloride intermediate was diluted with DCM (3 mL) and added slowly to a well-stirred mixture of 3-(2-aminoethyl)-1-methylpyridinium chloride hydrochloride (100 mg, 0.58 mmol) and K2CO3(178 mg, 1.29 mmol) in CH3CN (10 mL). After stirring 2 h, the reaction mixture was filtered and concentrated. The residue was purified by chromatography (10-20% MeOH/DCM) to afford the title compound as a solid (18 mg, 6%). 1H NMR (400 MHz, CDCl3) δ 9.13 (s, 1H), 8.77 (s, 1H), 8.40-8.32 (m, 1H), 8.03 (s, 1H), 7.71 (s, 1H), 7.51 (d, J=8.29 Hz, 1H), 7.15 (s, 1H), 6.96-6.78 (m, 3H), 6.62-6.38 (m, 5H), 4.54 (s, 3H), 4.03 (s, 2H), 3.77 (s, 4H), 3.52-3.41 (m, 4H), 3.22-3.12 (m, 2H), 1.82-1.58 (m, 6H), 1.50 (s, 7H), 1.21 (t, J=7.02 Hz, 4H); MS (EI) m/z 701 [M]+.

후처리

  1. concentrationconcentrated
  2. additiondiluted with DCM
  3. concentrationconcentrated to dryness
  4. additionThe sulfonyl chloride intermediate was diluted with DCM (3 mL)
  5. filtrationthe reaction mixture was filtered
  6. concentrationconcentrated
  7. customThe residue was purified by chromatography (10-20% MeOH/DCM)

출처 및 근거

ORD 기록
ord-5258a52d257c4192980ff1516c036004
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846739B2

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