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

HRID 533656ノート

反応式

HRID 533656 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-0b20f37117f74f14a87396a3dca8419c
出典データセット
uspto-grants-2014_10
特許番号
US08853238B2

反応ノート

読み込み中…