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

HRID 533656노트

반응식

HRID 533656 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-0b20f37117f74f14a87396a3dca8419c
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853238B2

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