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Diethyl Ether → HCID 10109822、化合物

HRID 1373806
ノート
印刷プレビュー

反応式

HRID 1373806 の反応式
Br[C:2]1[C:3]([C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)=[N:4][N:5]2[C:10]([NH:11][CH:12]3[CH2:16][CH2:15][CH2:14][CH2:13]3)=[CH:9][CH:8]=[CH:7][C:6]=12.[N:24]1[CH:29]=[CH:28][C:27](B(O)O)=[CH:26][CH:25]=1.C(=O)([O-])[O-].[Na+].[Na+].CCOCC>CN(C)C=O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH:12]1([NH:11][C:10]2[N:5]3[N:4]=[C:3]([C:17]4[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=4)[C:2]([C:27]4[CH:28]=[CH:29][N:24]=[CH:25][CH:26]=4)=[C:6]3[CH:7]=[CH:8][CH:9]=2)[CH2:16][CH2:15][CH2:14][CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 3283Diethyl EtherHCID 10340Sodium CarbonateHCID 2734379(Pyridin-4-yl)boronic acidHCID 69447740HCID 69447740、化合物

生成物 1

HCID 10109822HCID 10109822、化合物収率 46%

試薬・触媒・溶媒 2

HCID 178418476HCID 178418476、化合物
触媒
HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 3-bromo-N-cyclopentyl-2-(4-fluorophenyl)pyrazolo[1,5-α]pyridin-7-amine (106 mg, 0.28 mmol) in N,N-dimethylformamide (5 mL) was added 4-pyridinylboronic acid (70 mg, 0.56 mmol), sodium carbonate (0.28 mL, 2 M aqueous, 0.56 mmol) and dichlorobis(triphenylphosphine)palladium(II) (10 mg, 0.01 mmol). The resultant solution was heated to 100° C. for 18 hours. The reaction mixture 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 (2:1 hexanes:ether) provided N-cyclopentyl-2-(4-fluorophenyl)-3-(4-pyridinyl)pyrazolo[1,5-α]pyridin-7-amine (48 mg, 46%) as a yellow solid. 1H NMR (CDCl3): δ 8.50 (d, 2H), 7.53 (m, 2H), 7.22–7.18 (m, 3H), 7.06–6.97 (m, 3H), 6.00 (d, 1H), 5.95 (d, 1H), 3.99 (m, 1H), 2.16–2.08 (m, 2H), 1.83–1.66 (m, 6H); 13C NMR (CDCl3) δ 162.99 (d, JCF=246.6 Hz), 150.07, 149.98, 142.77, 141.98, 140.13, 131.02 (d, JCF=8.0 Hz), 129.04, 127.64, 123.98, 115.56 (d, JCF=21.2 Hz), 106.51, 102.22, 89.25, 53.88, 33.36, 24.05; 19F NMR (CDCl3) δ −113.49; MS m/z 373 (M+1).

後処理

  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

出典と根拠

ORDレコード
ord-cc14ae176cae421f8b6dad3eb76d9e08
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07163940B2

反応ノート

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