Pyridine → 6-Chloro-2-(ethylamino)pyridine-3-carbonyl fluoride

HRID 2207305노트

반응식

HRID 2207305 반응식
N1C=CC=CC=1.[F:7]N1N=C(F)C=C(F)N1.[Cl:16][C:17]1[CH:25]=[CH:24][C:20]([C:21](O)=[O:22])=[C:19]([NH:26][CH2:27][CH3:28])[N:18]=1>ClCCl>[Cl:16][C:17]1[CH:25]=[CH:24][C:20]([C:21]([F:7])=[O:22])=[C:19]([NH:26][CH2:27][CH3:28])[N:18]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 216944332,4,6-Trifluoro-1,2,3-triazineHCID 633764796-Chloro-2-(ethylamino)nicotinic acid

생성물 1

HCID 867145746-Chloro-2-(ethylamino)pyridine-3-carbonyl fluoride수율 99.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2 ml (24.8 mmol) of pyridine and 4.2 ml (49.8 mmol) of 2,4,6-trifluorotriazine were added to a suspension of 5.0 g (24.8 mmol) of 6-chloro-2-ethylamino-nicotinic acid in 125 ml of dichloromethane. The mixture was stirred for 3 hours at ambient temperature and then filtered. The solid was rinsed with 50 ml of dichloromethane and the filtrate was washed twice with 60 ml of ice-cold water. The organic phase was dried over Na2SO4 and the solvent was evaporated off under reduced pressure. 5.01 g of product were obtained in the form of an orange oil which was used without further purification.

후처리

  1. filtrationfiltered
  2. washThe solid was rinsed with 50 ml of dichloromethane
  3. washthe filtrate was washed twice with 60 ml of ice-cold water
  4. dry with materialThe organic phase was dried over Na2SO4
  5. customthe solvent was evaporated off under reduced pressure

출처 및 근거

ORD 기록
ord-892b107875144d8fb9d2bc4c30046293
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09376432B2

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