Chloroform → (3-Bromo-5-trifluoromethylsulfanylpyridine-2-yl)-methylamine

HRID 923812ノート

反応式

HRID 923812 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][C:10]([F:13])([F:12])[F:11])=[CH:5][N:4]=1.C(Cl)(Cl)Cl.[Br:18]N1C(=O)CCC1=O>O>[Br:18][C:8]1[C:3]([NH:2][CH3:1])=[N:4][CH:5]=[C:6]([S:9][C:10]([F:11])([F:13])[F:12])[CH:7]=1

参加物

5

反応物 3

HCID 6212ChloroformHCID 67184N-bromobutanimideHCID 67982149N-Methyl-5-((trifluoromethyl)thio)pyridin-2-amine

生成物 1

HCID 67981267(3-Bromo-5-trifluoromethylsulfanylpyridine-2-yl)-methylamine収率 93.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of methyl-(5-trifluoromethylsulfanylpyridine-2-yl)-amine (1.52 g) and chloroform (24 mL), N-bromosuccinimide (1.43 g) was added, and stirred at room temperature for 1 hour. Into the reaction mixture, water was poured, and extracted with chloroform. The combined organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography to give 1.96 g of (3-bromo-5-trifluoromethylsulfanylpyridine-2-yl)-methylamine.

後処理

  1. additionwas added
  2. extractionextracted with chloroform
  3. dry with materialThe combined organic layer was dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-bc32ec872325490e8ec1f33e7a87f95d
出典データセット
uspto-grants-2016_03
特許番号
US09278983B2

反応ノート

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