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Pyridine → 3-(6-Bromo-4-methyl-3,5-dioxo-4,5-dihydro-3H-[1,2,4]triazin-2-yl)-propionitrile

HRID 1917086
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HRID 1917086 반응식
[Br:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[C:5](=[O:8])[NH:6][N:7]=1.[C:11](#[N:14])[CH:12]=[CH2:13].N1C=CC=CC=1>O>[Br:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[C:5](=[O:8])[N:6]([CH2:13][CH2:12][C:11]#[N:14])[N:7]=1
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참가 물질

5

반응물 3

HCID 1049PyridineHCID 7855AcrylonitrileHCID 2605646-bromo-4-methyl-1,2,4-triazine-3,5(2h,4h)-dione

생성물 1

HCID 592988283-(6-Bromo-4-methyl-3,5-dioxo-4,5-dihydro-3H-[1,2,4]triazin-2-yl)-propionitrile수율 93%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2.4 g (11.6 mmol) of the triazine 2a and 7 mL (106 mmol) of acrylonitrile are placed in 24 mL of a solution of pyridine and water (1/1) under reflux for 3 h. After concentration, the reaction medium is extracted with AcOEt and then after drying on MgSO4, the organic phases are dry concentrated. After washing the obtained solid with ether, 2.8 g of intermediate 3a are obtained (yield=93%).

후처리

  1. temperatureunder reflux for 3 h
  2. concentrationAfter concentration
  3. extractionthe reaction medium is extracted with AcOEt
  4. customafter drying on MgSO4
  5. customthe organic phases are dry
  6. concentrationconcentrated
  7. washAfter washing the obtained solid with ether, 2.8 g of intermediate 3a
  8. customare obtained (yield=93%)

출처 및 근거

ORD 기록
ord-803a33367ddc4a929a00e38948010f7a
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08618287B2

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