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Cyclopentylamine → N-cyclopentyl-3-[2-(cyclopentylamino)-4-pyrimidinyl]-2-(3-methylphenyl)pyrazolo[1,5-a]pyridin-7-amine

HRID 861145
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HRID 861145 반응식
Cl[C:2]1[N:7]2[N:8]=[C:9]([C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([CH3:29])[CH:24]=3)[C:10]([C:11]3[CH:16]=[CH:15][N:14]=[C:13]([NH:17][CH:18]4[CH2:22][CH2:21][CH2:20][CH2:19]4)[N:12]=3)=[C:6]2[CH:5]=[CH:4][CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+].CCOCC.[CH:87]1([NH2:92])[CH2:91][CH2:90][CH2:89][CH2:88]1>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH:87]1([NH:92][C:2]2[N:7]3[N:8]=[C:9]([C:23]4[CH:28]=[CH:27][CH:26]=[C:25]([CH3:29])[CH:24]=4)[C:10]([C:11]4[CH:16]=[CH:15][N:14]=[C:13]([NH:17][CH:18]5[CH2:22][CH2:21][CH2:20][CH2:19]5)[N:12]=4)=[C:6]3[CH:5]=[CH:4][CH:3]=2)[CH2:91][CH2:90][CH2:89][CH2:88]1
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참가 물질

7

반응물 5

HCID 2906CyclopentylamineHCID 3283Diethyl EtherHCID 10796Cesium carbonateHCID 634876Binap, (A+-)-HCID 865967674-[7-chloro-2-(3-methylphenyl)pyrazolo[1,5-a]pyridin-3-yl]-N-cyclopentyl-2-pyrimidinamine

생성물 1

HCID 10297787
N-cyclopentyl-3-[2-(cyclopentylamino)-4-pyrimidinyl]-2-(3-methylphenyl)pyrazolo[1,5-a]pyridin-7-amine
수율 64%

시약·촉매·용매 1

HCID 167845palladium(II) acetate촉매

실험 절차

To a solution of 4-[7-chloro-2-(3-methylphenyl)pyrazolo[1,5-a]pyridin-3-yl]-N-cyclopentyl-2-pyrimidinamine (500 mg, 1.24 mmol) in cyclopentylamine (50 mL) was added successively racemic-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (308 mg, 0.49 mmol), cesium carbonate (0.81 g, 2.47 mmol) and palladium (II) acetate (70 mg, 0.31 mmol). The resultant mixture was heated to 95° C. for 18 hours at which time the reaction was judged complete by thin layer chromatography. The solution was cooled to room temperature and ether was added. The organic layer was washed with water and brine. The aqueous layer was extracted with ether and the combined organics dried over magnesium sulfate. Filtration and concentration, followed by flash chromatography (4:1 hexanes:ethyl acetate) provided N-cyclopentyl-3-[2-(cyclopentylamino)-4-pyrimidinyl]-2-(3-methylphenyl)pyrazolo[1,5-a]pyridin-7-amine (360 mg, 64%) as a yellow foam. 1H NMR (CDCl3) δ 7.94 (d, 1H), 7.79 (d, 1H), 7.46 (s, 1H), 7.40 (d, 1H), 7.34–7.29 (m, 2H), 7.24 (d, 1H), 6.27 (d, 1H), 6.03 (m, 2H), 5.12 (broad s, 1H), 4.35 (m, 1H), 3.99 (m, 1H), 2.40 (s, 3H), 2.14–2.04 (m, 4H), 1.81–1.52 (m, 12H); MS m/z 453 (M+1).

후처리

  1. washThe organic layer was washed with water and brine
  2. extractionThe aqueous layer was extracted with ether
  3. dry with materialthe combined organics dried over magnesium sulfate
  4. filtrationFiltration and concentration

출처 및 근거

ORD 기록
ord-5112672cbfa04abea08491bbe8be2eb5
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07153855B2

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