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

HRID 1043925

反応式

HRID 1043925 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-0e4a0e757bd349caa303e4b7767e4772
出典データセット
uspto-grants-2013_10
特許番号
US08563565B2

関連ノート

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