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

HRID 923792
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HRID 923792 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

To a mixture of N-methyl-(5-trifluoromethyl-pyridin-2-yl)-amine (17.3 g) and sulfuric acid (100 ml), nitric acid (12.3 g) was added drop-wise, and stirred with heating at 80° C. for 2 hours. The mixture was cooled to room temperature, and then the reaction mixture was poured into water. The precipitate was collected by filtration, washed with water, and dried under reduced pressure to give 18.8 g of N-methyl-(3-nitro-5-trifluoromethyl-pyridin-2-yl)-amine.

후처리

  1. additionwas added drop-wise
  2. temperatureThe mixture was cooled to room temperature
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-7ec808fd21c542bfbe744b8c65ea6091
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278983B2

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