Trifluoroacetic acid → N-(3'-fluoro-6'-methyl-2,2'-bipyridin-4-yl)-1H-pyrazolo[4,3-b]pyridin-7-amine

HRID 1522635ノート

反応式

HRID 1522635 の反応式
[F:1][C:2]1[C:3]([C:9]2[CH:14]=[C:13]([NH:15][C:16]3[CH:21]=[CH:20][N:19]=[C:18]4[CH:22]=[N:23][N:24](CC5C=CC(OC)=CC=5)[C:17]=34)[CH:12]=[CH:11][N:10]=2)=[N:4][C:5]([CH3:8])=[CH:6][CH:7]=1.FC1C(C2C=C(NC3C4C(=CN(CC5C=CC(OC)=CC=5)N=4)N=CC=3)C=CN=2)=NC(C)=CC=1.FC(F)(F)C(O)=O.C(=O)(O)[O-].[Na+]>ClCCl>[F:1][C:2]1[C:3]([C:9]2[CH:14]=[C:13]([NH:15][C:16]3[CH:21]=[CH:20][N:19]=[C:18]4[CH:22]=[N:23][NH:24][C:17]=34)[CH:12]=[CH:11][N:10]=2)=[N:4][C:5]([CH3:8])=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 67469529N-(3'-fluoro-6'-methyl-2,2'-bipyridin-4-yl)-2-(4-methoxybenzyl)-2H-pyrazolo[4,3-b]pyridin-7-amineHCID 67470402N-(3'-fluoro-6'-methyl-2,2'-bipyridin-4-yl)-1-(4-methoxybenzyl)-1H-pyrazolo[4,3-b]pyridin-7-amine

生成物 1

HCID 54670413N-(3'-fluoro-6'-methyl-2,2'-bipyridin-4-yl)-1H-pyrazolo[4,3-b]pyridin-7-amine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
70 °C

実験手順

N-(3′-Fluoro-6′-methyl-2,2′-bipyridin-4-yl)-1-(4-methoxybenzyl)-1H-pyrazolo[4,3-b]pyridin-7-amine and N-(3′-fluoro-6′-methyl-2,2′-bipyridin-4-yl)-2-(4-methoxybenzyl)-2H-pyrazolo[4,3-b]pyridin-7-amine and trifluoroacetic acid (20 mL) were combined and heated at 70° C. for 3 hours. The reaction mixture was then cooled, concentrated give a residue which was suspended in dichloromethane (50 mL) and added to a saturated solution of sodium bicarbonate (50 mL) with stirring. The mixture was sonicated and filtered. The solid was dried under vacuum and suspended in ethyl acetate. The solid again collected by filtration to give N-(3′-fluoro-6′-methyl-2,2′-bipyridin-4-yl)-1H-pyrazolo[4,3-b]pyridin-7-amine. MS [M+H] found 321.3.

後処理

  1. temperatureThe reaction mixture was then cooled
  2. concentrationconcentrated
  3. customgive a residue which
  4. customThe mixture was sonicated
  5. filtrationfiltered
  6. customThe solid was dried under vacuum
  7. filtrationThe solid again collected by filtration

出典と根拠

ORDレコード
ord-1b1bc0356e744540bdd6a5da91d36d21
出典データセット
uspto-grants-2015_07
特許番号
US09073918B2

反応ノート

読み込み中…