Chloroform → HCID 15614715, 화합물

HRID 477648노트

반응식

HRID 477648 반응식
[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

참가 물질

3

반응물 2

HCID 6212Chloroform2회HCID 156147143-(4-Fluorobenzylamino)-4-nitropyridine

생성물 1

HCID 15614715HCID 15614715, 화합물

실험 절차

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 one 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 13).

후처리

  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

출처 및 근거

ORD 기록
ord-60823f941e484dedb5cff085cb0583cd
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04888426

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