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

HRID 633557ノート

反応式

HRID 633557 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 60C (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 and partitioned into ethyl acetate and cold water. The organic layer was washed with saturated aqueous sodium chloride, dried (anhydrous 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 (anhydrous Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-cf4598693ca34dc095286c6837bfb2c1
出典データセット
uspto-grants-2016_04
特許番号
US09321764B2

反応ノート

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