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Potassium Carbonate → HCID 10142490, 화합물

HRID 861126
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HRID 861126 반응식
Br[C:2]1[CH:3]=[C:4]([C:8]2[C:22]([C:23]3[CH:28]=[CH:27][N:26]=[C:25]([NH:29][CH:30]4[CH2:34][CH2:33][CH2:32][CH2:31]4)[N:24]=3)=[C:11]3[CH:12]=[CH:13][CH:14]=[C:15]([NH:16][CH:17]4[CH2:21][CH2:20][CH2:19][CH2:18]4)[N:10]3[N:9]=2)[CH:5]=[CH:6][CH:7]=1.[C:35]1(B(O)O)[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1.C(=O)([O-])[O-].[K+].[K+].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>CN(C)C=O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O.C(OCC)(=O)C>[C:2]1([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH:7]=[CH:6][CH:5]=[C:4]([C:8]2[C:22]([C:23]3[CH:28]=[CH:27][N:26]=[C:25]([NH:29][CH:30]4[CH2:34][CH2:33][CH2:32][CH2:31]4)[N:24]=3)=[C:11]3[CH:12]=[CH:13][CH:14]=[C:15]([NH:16][CH:17]4[CH2:21][CH2:20][CH2:19][CH2:18]4)[N:10]3[N:9]=2)[CH:3]=1
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참가 물질

9

반응물 4

HCID 11430Potassium CarbonateHCID 11776TriphenylphosphineHCID 66827Phenylboronic AcidHCID 10142612HCID 10142612, 화합물

생성물 1

HCID 10142490HCID 10142490, 화합물수율 89%

시약·촉매·용매 4

HCID 167845palladium(II) acetate
촉매
HCID 962Water용매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

To a solution of 2-(3-bromophenyl)-N-cyclopentyl-3-[2-(cyclopentylamino)-4-pyrimidinyl]pyrazolo[1,5-a]pyridin-7-amine (100 mg, 0.19 mmol) in dimethylformamide (6 mL) was added phenylboronic acid (47 mg, 0.39 mmol), palladium (II) acetate (4.3 mg, 0.02 mmol), potassium carbonate (54 mg, 0.39 mmol) and triphenyl phosphine (30 mg, 0.08 mmol). The reaction was heated at 100° C. for 24 hours. After allowing the reaction mixture to cool to room temperature, ethyl acetate and water were added. The organic layer was separated and washed with water, then brine and dried (magnesium sulfate). Filtration and concentration, followed by purification with flash chromatography (4:6 ethyl acetate:hexanes) gave 2-[1,1′-biphenyl]-3-yl-N-cyclopentyl-3-[2-(cyclopentylamino)-4-pyrimidinyl]pyrazolo[1,5-a]pyridin-7-amine as a yellow foam (87 mg, 89%). 1H NMR (CDCl3): δ 8.01 (d, 1H), 7.92 (s, 1H), 7.81 (d, 1H), 7.69–7.62 (m, 4H), 7.53 (t, 1H), 7.47–7.43 (m, 2H), 7.38–7.32 (m, 2H), 6.40 (d, 1H), 6.09–6.05 (m, 2H), 5.16 (m, 1H), 4.37 (m, 1H), 4.03 (m, 1H), 2.15–2.06 (m, 4H), 1.82–1.64 (m, 12H); MS m/z 515 (M+1).

후처리

  1. temperatureto cool to room temperature
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materialbrine and dried (magnesium sulfate)
  5. filtrationFiltration and concentration
  6. customfollowed by purification with flash chromatography (4:6 ethyl acetate:hexanes)

출처 및 근거

ORD 기록
ord-6e8d1c3ab2894304a8f41b5c835d4ba4
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07153855B2

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