Ammonium Chloride → 3-bromo-N-methyl-5-(trifluoromethyl)pyridin-2-amine

HRID 923794ノート

反応式

HRID 923794 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][N:4]=1.[Br:13]N1C(=O)CCC1=O.[Cl-].[NH4+]>CN(C=O)C>[CH3:1][NH:2][C:3]1[C:8]([Br:13])=[CH:7][C:6]([C:9]([F:12])([F:10])[F:11])=[CH:5][N:4]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 67184N-bromobutanimideHCID 18526206N-Methyl-5-(trifluoromethyl)pyridin-2-amine

生成物 1

HCID 679813233-bromo-N-methyl-5-(trifluoromethyl)pyridin-2-amine収率 95.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of N-methyl-(5-trifluoromethyl-pyridin-2-yl)-amine (3.48 g) and DMF (20 ml), N-bromosuccinimide (4.27 g) was added, and stirred at room temperature for 1 hour. Into the reaction mixture, saturated aqueous ammonium chloride solution was poured, and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography to give 4.8 g of N-methyl-(3-bromo-5-trifluoromethyl-pyridin-2-yl)-amine.

後処理

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

出典と根拠

ORDレコード
ord-ae2d8eac312e462f8f7915a32a8e413d
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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