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Benzene → HCID 59632205, 화합물

HRID 2369107
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HRID 2369107 반응식
[CH2:1]([NH:3][C:4]([C:6]1[CH:10]=[C:9]([C:11]2[S:12][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([S:22]([CH3:25])(=[O:24])=[O:23])[CH:17]=3)=[CH:14][CH:15]=2)[N:8]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[Cl:32])[N:7]=1)=O)[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:42])=CC=1.C1(C)C=CC=CC=1.C1C=CC=CC=1>CCOCC>[CH2:1]([NH:3][C:4]([C:6]1[CH:10]=[C:9]([C:11]2[S:12][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([S:22]([CH3:25])(=[O:24])=[O:23])[CH:17]=3)=[CH:14][CH:15]=2)[N:8]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[Cl:32])[N:7]=1)=[S:42])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 241BenzeneHCID 1140TolueneHCID 87949Lawesson's reagentHCID 59633427HCID 59633427, 화합물

생성물 1

HCID 59632205HCID 59632205, 화합물수율 38%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a dry, N2 purged 50 mL round bottom flask attached with condenser was added 1-(2-Chloro-phenyl)-5-[5-(3-methanesulfonyl-phenyl)-thiophen-2-yl]-1H-pyrazole-3-carboxylic acid ethylamide (100 mg, 206 μmol), Lawesson's reagent (200 mg, 494 μmol), and anhydrous toluene (8 mL). The reaction solution was allowed to stir at reflux for 14 hrs. The reaction solution was allowed to cool to room temperature prior to addition of a 1:1 mixture of benzene and Et2O. The resulting precipitate was removed by vacuum filtration through a Buchner funnel. The filtrate was concentrated on the Rotavapor and the crude residue was chromatographed through a 12 g SiO2 column using a mobile phase gradient of 100% Hx to 50% EtOAc to afford 39 mg (38% yield) of the title compound. 1H NMR (400 MHz, CDCl3) δ 8.68 (br s, 1H), 8.02 (s, 1H), 7.83 (d, 1H), 7.72 (d, 1H), 7.48-7.70 (m, 5H), 7.42 (s, 1H), 7.22 (d, 1H), 6.83 (d, 1H), 3.87 (m, 2H), 3.07 (s, 3H), 1.36 (t, 3H). MS (ES) 502.3, 504.3 [M+H]+.

후처리

  1. customTo a dry, N2 purged 50 mL round bottom flask
  2. customattached with condenser
  3. temperatureat reflux for 14 hrs
  4. customThe resulting precipitate was removed by vacuum filtration through a Buchner funnel
  5. concentrationThe filtrate was concentrated on the Rotavapor
  6. customthe crude residue was chromatographed through a 12 g SiO2 column

출처 및 근거

ORD 기록
ord-b9732f709f7b4d4cb7649db2410f349c
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703805B2

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