Nitric Acid → HCID 178418402、化合物

HRID 2155

反応式

HRID 2155 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178418402HCID 178418402、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-dd9f79aff70f4e008da6da583aa08a55
出典データセット
uspto-grants-1998_03
特許番号
US05728708

関連ノート

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