Chloroacetyl chloride → 2-chloro-1-(4-(5-(1-methyl-1H-1,2,4-triazol-3-yl)pyridin-2-yl)-5,6-dihydropyridin-1(2H)-yl)ethanone

HRID 1020963ノート

反応式

HRID 1020963 の反応式
[OH-].[Na+].[Cl:3][CH2:4][C:5](Cl)=[O:6].Cl.Cl.[CH3:10][N:11]1[CH:15]=[N:14][C:13]([C:16]2[CH:17]=[CH:18][C:19]([C:22]3[CH2:23][CH2:24][NH:25][CH2:26][CH:27]=3)=[N:20][CH:21]=2)=[N:12]1>C(Cl)Cl.O>[Cl:3][CH2:4][C:5]([N:25]1[CH2:24][CH2:23][C:22]([C:19]2[CH:18]=[CH:17][C:16]([C:13]3[N:14]=[CH:15][N:11]([CH3:10])[N:12]=3)=[CH:21][N:20]=2)=[CH:27][CH2:26]1)=[O:6]

参加物

6

反応物 3

HCID 6577Chloroacetyl chlorideHCID 14798Sodium HydroxideHCID 673440865-(1-methyl-1H-1,2,4-triazol-3-yl)-2-(1,2,3,6-tetrahydropyridin-4-yl)pyridine dihydrochloride

生成物 1

HCID 583719992-chloro-1-(4-(5-(1-methyl-1H-1,2,4-triazol-3-yl)pyridin-2-yl)-5,6-dihydropyridin-1(2H)-yl)ethanone収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒3 回

反応条件

温度
0 °C

実験手順

Added 1N NaOH (50 ml, 50 mmol) and Chloroacetyl chloride (3 ml, 37.7 mmol) in CH2Cl2 (50 ml) dropwise to a solution of 5-(1-methyl-1H-1,2,4-triazol-3-yl)-2-(1,2,3,6-tetrahydropyridin-4-yl)pyridine dihydrochloride (5BX) (1 g, 3.60 mmol) in CH2Cl2 (50 ml at 0° C., maintaining pH at >12. Mixture was stirred for 2 hours at 0° C., then reaction was diluted with CH2Cl2 (200 ml) and H2O (100 ml). The organic layer was separated, washed with H2O (50 ml), dried (Na2SO4), filtered and solvent evaporated yielding title product as a white solid (1.1 g, 100%) MS (MH, 318)

後処理

  1. temperaturemaintaining pH at >12
  2. customreaction
  3. customThe organic layer was separated
  4. washwashed with H2O (50 ml)
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customsolvent evaporated

出典と根拠

ORDレコード
ord-a4236ca36aa54877b96952a97071e7ae
出典データセット
uspto-grants-2014_05
特許番号
US08716483B2

反応ノート

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