Sodium methanethiolate → 3-Bromo-2-(2,4-difluorophenoxy)-5-(methylthiomethyl)pyridine

HRID 930936ノート

反応式

HRID 930936 の反応式
[Br:1][C:2]1[C:3]([O:10][C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=2[F:18])=[N:4][CH:5]=[C:6]([CH2:8]Br)[CH:7]=1.[CH3:19][S-:20].[Na+]>CN(C)C=O>[Br:1][C:2]1[C:3]([O:10][C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=2[F:18])=[N:4][CH:5]=[C:6]([CH2:8][S:20][CH3:19])[CH:7]=1

参加物

4

反応物 2

HCID 4378561Sodium methanethiolateHCID 867210763-Bromo-5-(bromomethyl)-2-(2,4-difluorophenoxy)pyridine

生成物 1

HCID 867210773-Bromo-2-(2,4-difluorophenoxy)-5-(methylthiomethyl)pyridine収率 96.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The product from Example 311c (0.75 g, 1.979 mmol) and sodium thiomethoxide (0.139 g, 1.979 mmol) were combined in dimethylformamide (3.96 mL), stirred for 4 hours at ambient temperature, and partitioned into ethyl acetate and cold water. The organic layer was washed with saturated aqueous sodium chloride, dried (Na2SO4), filtered, and concentrated to afford the title compound (0.66 g, 96%).

後処理

  1. custompartitioned into ethyl acetate and cold water
  2. washThe organic layer was washed with saturated aqueous sodium chloride
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-392c5e1d80c748c29dac0e5e9e1e4d5c
出典データセット
uspto-grants-2016_03
特許番号
US09296741B2

反応ノート

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