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

HRID 1750052노트

반응식

HRID 1750052 반응식
[Br:1]N1C(=O)CCC1=O.[CH3:9][NH:10][C:11]1[CH:16]=[CH:15][C:14]([S:17][C:18]([F:21])([F:20])[F:19])=[CH:13][N:12]=1.C(Cl)(Cl)Cl>O>[Br:1][C:16]1[C:11]([NH:10][CH3:9])=[N:12][CH:13]=[C:14]([S:17][C:18]([F:19])([F:21])[F:20])[CH:15]=1

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.43 g of N-bromosuccinimide was added to a mixture of 1.52 g of methyl-(5-trifluoromethylsulfanylpyridin-2-yl)-amine and 24 ml of chloroform, and the mixture was stirred at room temperature for 1 hour. Water was added to the reaction mixture, and the mixture was extracted with chloroform. The combined organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 1.96 g of (3-bromo-5-trifluoromethylsulfanylpyridin-2-yl)-methylamine.

후처리

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1c018e04ea034546a5b707024be217be
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09156838B2

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