Nitric Acid → HCID 178418402, 화합물

HRID 2155

반응식

HRID 2155 반응식
[N:1]#[C:2][NH2:3].[F:4][C:5]([F:14])([F:13])[C:6]1[CH:7]=[C:8]([CH:10]=[CH:11][CH:12]=1)[NH2:9].[N+:15]([O-:18])([OH:17])=[O:16]>C(O)C>[N+:15]([O-:18])([OH:17])=[O:16].[F:4][C:5]([F:13])([F:14])[C:6]1[CH:7]=[C:8]([NH:9][C:2]([NH2:3])=[NH:1])[CH:10]=[CH:11][CH:12]=1

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 73753-(Trifluoromethyl)anilineHCID 9864Cyanamide

생성물 1

HCID 178418402HCID 178418402, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

6.3 g (150 mmol) of cyanamide (50% in water) are added to a suspension of 16.1 g (100 mmol) of 3-trifluoromethyl-aniline in 35 ml of ethanol. 7.0 ml of nitric acid (65%, 0.1 mol) are then added to the brown solution and the reaction mixture is heated for 20 h under RF. It is then cooled to 0° and filtered, and the material retained on the filter is washed with ethanol and dried at 60° under HV to give 3-trifluoromethyl-phenylguanidine nitrate; 1H-NMR (dimethyl sulfoxide): 7.6 (7H,m), 9.9 (1H,br,s).

후처리

  1. temperaturethe reaction mixture is heated for 20 h under RF
  2. temperatureIt is then cooled to 0°
  3. filtrationfiltered
  4. washis washed with ethanol
  5. customdried at 60° under HV

출처 및 근거

ORD 기록
ord-dd9f79aff70f4e008da6da583aa08a55
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728708

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