Sodium Sulfate → 2-(Difluoromethoxy)-4-iodo-3,5-dimethylpyridine

HRID 1043925

반응식

HRID 1043925 반응식
[I:1][C:2]1[C:7]([CH3:8])=[CH:6][N:5]=[C:4]([OH:9])[C:3]=1[CH3:10].FS([C:15]([F:20])([F:19])C(O)=O)(=O)=O.S([O-])([O-])(=O)=O.[Na+].[Na+].C(=O)(O)[O-].[Na+]>C(#N)C>[F:19][CH:15]([F:20])[O:9][C:4]1[C:3]([CH3:10])=[C:2]([I:1])[C:7]([CH3:8])=[CH:6][N:5]=1

참가 물질

6

반응물 4

HCID 24436Sodium SulfateHCID 516892Sodium BicarbonateHCID 27375162,2-Difluoro-2-(fluorosulfonyl)acetic acidHCID 178430689HCID 178430689, 화합물

생성물 1

HCID 866863482-(Difluoromethoxy)-4-iodo-3,5-dimethylpyridine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

4-iodo-3,5-dimethylpyridin-2-ol (350 mg), 2-(fluorosulfonyl)difluoroacetic acid (0.17 mL), and sodium sulfate (39.9 mg) were added to acetonitrile (5.7 mL). The mixture was stirred at room temperature for 3.5 hours. A saturated aqueous sodium bicarbonate solution was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was concentrated under reduced pressure to give the title compound (378.6 mg).

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. concentrationThe organic layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0e4a0e757bd349caa303e4b7767e4772
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563565B2

연결된 노트

불러오는 중…