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Potassium Carbonate → HCID 10173307, 화합물

HRID 1296727
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HRID 1296727 반응식
CN(C)/[CH:3]=[CH:4]/[C:5]([C:7]1[C:8]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)=[N:9][N:10]2[C:15]=1[CH:14]=[CH:13][N:12]=[C:11]2[S:16][CH3:17])=O.Cl.[CH:27]1([NH:32][C:33]([NH2:35])=[NH:34])[CH2:31][CH2:30][CH2:29][CH2:28]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.O>[CH:27]1([NH:32][C:33]2[N:35]=[C:5]([C:7]3[C:8]([C:18]4[CH:19]=[CH:20][C:21]([F:24])=[CH:22][CH:23]=4)=[N:9][N:10]4[C:15]=3[CH:14]=[CH:13][N:12]=[C:11]4[S:16][CH3:17])[CH:4]=[CH:3][N:34]=2)[CH2:31][CH2:30][CH2:29][CH2:28]1
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6

반응물 3

HCID 11430Potassium CarbonateHCID 69449408HCID 69449408, 화합물HCID 178479367HCID 178479367, 화합물

생성물 1

HCID 10173307HCID 10173307, 화합물수율 32%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

To a solution of (2E)-3-(dimethylamino)-1-[2-(4-fluorophenyl)-7-(methylsulfanyl)pyrazolo[1,5-c]pyrimidin-3-yl]prop-2-en-1-one (660 mg, 1.85 mmol) and N-cyclopentylguanidine hydrochloride (600 mg, 3.71 mmol) in N,N-dimethylformamide (10 mL) was added potassium carbonate (760 mg, 5.55 mmol). The reaction mixture was heated to 100° C. for 1 hour and then to 115° C. for 4 hours. The reaction was allowed to cool to room temperature and diluted with water. The mixture was extracted with ethyl acetate, washed with brine, dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel chromatography eluting with 50% acetone in dichloromethane to yield N-cyclopentyl-4-[2-(4-fluorophenyl)-7-(methylsulfanyl)pyrazolo[1,5-c]pyrimidin-3-yl]pyrimidin-2-amine (210 mg, 32%). 1H NMR (CDCl3): δ 8.05(d,1H), 7.94 (m, 2H), 7.64 (dd, 2H), 7.13 (t, 2H), 6.29 (d, 1H), 5.21 (bs, 1H), 4.31 (m, 1H), 2.72 (s, 3H), 2.06 (m, 2H), 1.49–1.82 (m, 6H). MS m/z 421 (M+1).

후처리

  1. temperatureto cool to room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. washwashed with brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified
  8. washeluting with 50% acetone in dichloromethane

출처 및 근거

ORD 기록
ord-d35b582d94884a9bb322f8eed1017e19
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07247626B2

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