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Cyclopentylamine → HCID 69447740、化合物

HRID 1373805
ノート
印刷プレビュー

反応式

HRID 1373805 の反応式
[Br:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)=[N:4][N:5]2[C:10](Cl)=[CH:9][CH:8]=[CH:7][C:6]=12.C(=O)([O-])[O-].[Cs+].[Cs+].[CH:25]1([NH2:30])[CH2:29][CH2:28][CH2:27][CH2:26]1.CCOCC>C1(C)C=CC=CC=1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1>[Br:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)=[N:4][N:5]2[C:10]([NH:30][CH:25]3[CH2:29][CH2:28][CH2:27][CH2:26]3)=[CH:9][CH:8]=[CH:7][C:6]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 2906CyclopentylamineHCID 3283Diethyl EtherHCID 10796Cesium carbonateHCID 86616860HCID 86616860、化合物

生成物 1

HCID 69447740HCID 69447740、化合物収率 83%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒
HCID 634876
Binap, (A+-)-
触媒
HCID 1140Toluene溶媒

実験手順

To a solution of 3-bromo-7-chloro-2-(4-fluorophenyl)pyrazolo[1,5-α]pyridine (1.26 g, 3.9 mmol) in toluene (39 mL) was added successively racemic-BINAP (153 mg, 0.23 mmol), cesium carbonate (1.44 g, 3.9 mmol), cyclopentylamine (1.14 mL, 11.5 mmol), and palladium (II) acetate (35 mg, 0.15 mmol). The resultant mixture was heated at 95° C. for 2.5 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 (100:1 to 40:1 hexanes:ether) provided 3-bromo-N-cyclopentyl-2-(4-fluorophenyl)pyrazolo[1,5-α]pyridin-7-amine (1.2 g, 83%) as a white crystalline solid upon standing. 1H NMR (CDCl3): δ 8.05 (dd, 2H), 7.22–7.14 (m, 3H), 6.87 (d, 1H), 5.95–5.92 (m, 2H), 4.00 (m, 1H). 2.13 (m, 2H), 1.84–1.67 (m, 6H); 19F NMR (CDCl3) δ −113.44; MS m/z 374 (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-1085a181c4ba42f8a5771b6598293385
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

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート