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2-Chloro-4,6-dimethyl-3-pyridinecarbonitrile → 4,6-Dimethylnicotinonitrile

HRID 1450253
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HRID 1450253 반응식
Cl[C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH3:10])[CH:5]=[C:4]([CH3:11])[N:3]=1.[Sn]>Cl.O>[C:8]([C:7]1[C:6]([CH3:10])=[CH:5][C:4]([CH3:11])=[N:3][CH:2]=1)#[N:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2232612-Chloro-4,6-dimethyl-3-pyridinecarbonitrileHCID 5352426Tin atom

생성물 1

HCID 2439174,6-Dimethylnicotinonitrile수율 54%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

실험 절차

23 g of 2-chloro-3-cyano-4,6-dimethylpyridine are dissolved in 185 ml of concentrated hydrochloric acid and 240 ml of water. 25.4 g of tin metal are added and the mixture is brought to 100° C. The reaction is monitored by thin layer chromatography (TLC). When the reaction is complete, the mixture is allowed to return to room temperature and filtered and the filtrate is neutralized using sodium hydroxide solution. The mixture is extracted with methylene chloride and the combined organic phases are washed with saturated aqueous sodium bicarbonate solution and dried over anhydrous magnesium sulphate. The solution is concentrated to give 5-cyano-2,4-dimethylpyridine in the form of a yellow precipitate.

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후처리

  1. customis brought to 100° C
  2. customto return to room temperature
  3. filtrationfiltered
  4. extractionThe mixture is extracted with methylene chloride
  5. washthe combined organic phases are washed with saturated aqueous sodium bicarbonate solution
  6. dry with materialdried over anhydrous magnesium sulphate
  7. concentrationThe solution is concentrated

출처 및 근거

ORD 기록
ord-0db64533d23a4e5888a937cbca11d533
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05602132

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