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 1020963노트

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HRID 1020963 반응식
[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]

참가 물질

6

반응물 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

생성물 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)ethanone수율 100%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매3회

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온도
0 °C

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-a4236ca36aa54877b96952a97071e7ae
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716483B2

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