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

HRID 533654
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HRID 533654 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 dropwise, 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 dropwise
  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-d39fbe9c1f5a46bfa52cb953a9d95461
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08853238B2

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