Chloroform → HCID 15614715、化合物

HRID 280328ノート

反応式

HRID 280328 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][C:15]=2[N+:16]([O-:18])=[O:17])=[CH:4][CH:3]=1.[Cl:19]C(Cl)Cl>>[ClH:19].[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][NH:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][C:15]=2[N+:16]([O-:18])=[O:17])=[CH:6][CH:7]=1

参加物

3

反応物 2

HCID 6212Chloroform2 回HCID 156147143-(4-Fluorobenzylamino)-4-nitropyridine

生成物 1

HCID 15614715HCID 15614715、化合物

実験手順

To a stirred and cooled (0° C.) solution of 8.7 parts of N-[(4-fluorophenyl)methyl]-4-nitro-3-pyridinamine, 1-oxide and 150 parts of trichloromethane was added dropwise a solution of 10.2 parts of phosphor trichloride in 75 parts of trichloromethane. Upon completion, the mixture was allowed to reach room temperature and stirring was continued for 1 hour at reflux temperature. The reaction mixture was cooled and the solvent was evaporated. The residue was stirred in trichloromethane. The product was filtered off and dried, yielding 9 parts of N-[(4-fluorophenyl)methyl]-4-nitro-3-pyridinamine monohydrochloride (7).

後処理

  1. customto reach room temperature
  2. stirringstirring
  3. temperatureat reflux temperature
  4. temperatureThe reaction mixture was cooled
  5. customthe solvent was evaporated
  6. stirringThe residue was stirred in trichloromethane
  7. filtrationThe product was filtered off
  8. customdried

出典と根拠

ORDレコード
ord-f03406e695534c4ab96f8a8c90623eef
出典データセット
uspto-grants-1986_05
特許番号
US04588722

反応ノート

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