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Potassium Carbonate → HCID 86618782、化合物

HRID 1157569
ノート
印刷プレビュー

反応式

HRID 1157569 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([CH:8]=[CH:9][C:10]2[CH:11]=[C:12]([NH:16][C:17](=[O:22])[C:18]([F:21])([F:20])[F:19])[CH:13]=[CH:14][CH:15]=2)[CH:5]=[CH:4][N:3]=1.[N+]([O-])([O-])=O.[NH2:27][N+:28]1[CH:33]=[CH:32][CH:31]=[C:30]([F:34])[CH:29]=1.C([O-])([O-])=O.[K+].[K+].[Li+].[Cl-]>CN(C=O)C>[Cl:1][C:2]1[N:7]=[C:6]([C:8]2[C:9]([C:10]3[CH:11]=[C:12]([NH:16][C:17](=[O:22])[C:18]([F:19])([F:20])[F:21])[CH:13]=[CH:14][CH:15]=3)=[N:27][N:28]3[CH:29]=[C:30]([F:34])[CH:31]=[CH:32][C:33]=23)[CH:5]=[CH:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 433294Lithium ChlorideHCID 686441961-Amino-3-fluoropyridinium nitrateHCID 86631082N-[3-(2-Chloro-pyrimidin-4-ylethenyl)-phenyl]-2,2,2-trifluoro-acetamide

生成物 1

HCID 86618782HCID 86618782、化合物収率 30.1%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒
2 回

実験手順

To a solution of N-[3-(2-chloro-pyrimidin-4-ylethenyl)-phenyl]-2,2,2-trifluoro-acetamide (See Example 1, step B) (5.0 g) in DMF (40 mL) were added 1-amino-3-fluoropyridinium nitrate (5.4 g) and K2CO3 (6.0 g). The reaction was kept stirring at RT for 1.5 h. The DMF solution was poured into 5% LiCl solution (60 mL) and extracted with EtOAc (2×30 mL). The combined organic phase were dried (Na2SO4) and concentrated. The crude products were separated through silica gel column chromatography to afford two products. The first to elute was N-{3-[3-(2-chloro-4-pyrimidinyl)-6-fluoropyrazolo[1,5-a]pyridin-2-yl]phenyl}-2,2,2-trifluoroacetamide (2.0 g, 30% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 7.08 (d, 1H, J=5.49 Hz), 7.45 (d, 1H, J=7.68 Hz), 7.55 (t, 1H, J=7.96 Hz), 7.73-7.79 (m, 1H), 7.83 (d, 1H, J=0.91 Hz), 7.95 (t, 1H, J=1.74 Hz), 8.41 (dd, 1H, J=9.97, 5.76 Hz), 8.49 (d, 1H, J=5.49 Hz), 9.27 (dd, 1H, J=4.30, 2.29 Hz). ES-LC/MS m/z=436 [M+H]+.

後処理

  1. extractionextracted with EtOAc (2×30 mL)
  2. dry with materialThe combined organic phase were dried (Na2SO4)
  3. concentrationconcentrated
  4. customThe crude products were separated through silica gel column chromatography
  5. customto afford two products
  6. washThe first to elute

出典と根拠

ORDレコード
ord-edf44eb9edda47d2bfec6c05a57066e1
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07807673B2

反応ノート

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