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Nitric Acid → N-Methyl-3-nitro-5-(trifluoromethyl)pyridin-2-amine

HRID 1256614
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HRID 1256614 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.S(=O)(=O)(O)O.[N+:18]([O-])([OH:20])=[O:19]>O>[CH3:1][NH:2][C:3]1[C:8]([N+:18]([O-:20])=[O:19])=[CH:7][C:6]([C:9]([F:12])([F:10])[F:11])=[CH:5][N:4]=1
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참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 18526206N-Methyl-5-(trifluoromethyl)pyridin-2-amine

생성물 1

HCID 2775319N-Methyl-3-nitro-5-(trifluoromethyl)pyridin-2-amine수율 86.6%

시약·촉매·용매 1

HCID 962Water용매

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온도
80 °C

실험 절차

Into a mixture of 17.3 g of N-methyl(5-trifluoromethylpyridin-2-yl)-amine and 100 ml of sulfuric acid was dropped 12.3 g of nitric acid, then, the mixture was stirred for 2 hours while heating at 80° C. After cooling down to room temperature, water was poured into the reaction mixture, and the deposited precipitate was filtrated, then, washed with water, then, dried under reduced pressure to obtain 18.8 g of N-methyl(3-nitro-5-trifluoromethylpyridin-2-yl)-amine.

후처리

  1. temperatureAfter cooling down to room temperature
  2. filtrationthe deposited precipitate was filtrated
  3. washwashed with water
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-5847bb67d5674dbbbe148653720d92df
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461181B2

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