Chloroform → HCID 15614715、化合物

HRID 637398ノート

反応式

HRID 637398 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 (intermediate 17).

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-32097ff553c64ba3babd1617b2e26c01
出典データセット
uspto-grants-1985_12
特許番号
US04556660

反応ノート

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