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Water → N-{4-[5-chloro-7-(cyclopentylamino)-2-(4-fluorophenyl)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinyl}-N-cyclopentylamine

HRID 1062870
ノート
印刷プレビュー

反応式

HRID 1062870 の反応式
[CH:1]1([NH:6][C:7]2[N:12]=[C:11]([C:13]3[C:14]([C:24]4[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=4)=[N:15][N:16]4[C:21](Cl)=[CH:20][C:19]([Cl:23])=[CH:18][C:17]=34)[CH:10]=[CH:9][N:8]=2)[CH2:5][CH2:4][CH2:3][CH2:2]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+].O.[CH:84]1([NH2:89])[CH2:88][CH2:87][CH2:86][CH2:85]1>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:23][C:19]1[CH:20]=[C:21]([NH:89][CH:84]2[CH2:88][CH2:87][CH2:86][CH2:85]2)[N:16]2[N:15]=[C:14]([C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=3)[C:13]([C:11]3[CH:10]=[CH:9][N:8]=[C:7]([NH:6][CH:1]4[CH2:5][CH2:4][CH2:3][CH2:2]4)[N:12]=3)=[C:17]2[CH:18]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 962WaterHCID 2906CyclopentylamineHCID 10796Cesium carbonateHCID 634876Binap, (A+-)-HCID 10203732N-cyclopentyl-4-[5,7-dichloro-2-(4-fluorophenyl)pyrazolo(1,5-a]pyridin-3-yl]-2-pyrimidinamine

生成物 1

HCID 10278127
N-{4-[5-chloro-7-(cyclopentylamino)-2-(4-fluorophenyl)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinyl}-N-cyclopentylamine
収率 68%

試薬・触媒・溶媒 1

HCID 167845palladium(II) acetate触媒

反応条件

温度
80 °C

実験手順

To a solution of N-cyclopentyl-4-[5,7-dichloro-2-(4-fluorophenyl)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinamine (0.04 g, 0.1 mmol) in cyclopentylamine (4 mL) was added racemic-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (25 mg), cesium carbonate (50 mg) and palladium (II) acetate (5 mg). The resulting mixture was stirred at 80° C. for 24 hours. Water was added and the mixture was extracted with ethyl acetate. The ethyl acetate phase was washed with brine, dried (magnesium sulfate), filtered and concentrated in vacuo. The resulting residue was purified by flash chromatography (3:7 ethyl acetate-hexane) to give 30 mg (68%) of N-{4-[5-chloro-7-(cyclopentylamino)-2-(4-fluorophenyl)pyrazolo[1,5-a]pyridin-3-yl]-2-pyrimidinyl}-N-cyclopentylamine as a yellow foam. 1H NMR (CDCl3): δ 8.00 (d, 1H), 7.82 (s, 1H), 7.61 (m, 2H), 7.15 (t, 2H), 6.23 (d, 1H), 6.06 (d, 1H), 6.00 (s, 1H), 5.11 (d, 1H), 4.35 (m, 1H), 3.95 (m, 1H), 2.0-2.1 (m, 4H), 1.5-1.9 (m, 12H); 19F NMR (CDCl3): δ−113.0; MS m/z 491 (M+1).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate phase was washed with brine
  3. dry with materialdried (magnesium sulfate)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe resulting residue was purified by flash chromatography (3:7 ethyl acetate-hexane)

出典と根拠

ORDレコード
ord-4151671384c24cb3add79baf4e473157
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06962914B2

反応ノート

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