Diphosgene → 2-Fluoro-1-isocyanato-4-methoxybenzene

HRID 257361노트

반응식

HRID 257361 반응식
[F:1][C:2]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:3]=1[NH2:4].Cl[C:12](OC(Cl)(Cl)Cl)=[O:13]>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:3]=1[N:4]=[C:12]=[O:13]

참가 물질

4

반응물 2

HCID 10426DiphosgeneHCID 37563832-Fluoro-4-methoxyaniline

생성물 1

HCID 189810662-Fluoro-1-isocyanato-4-methoxybenzene

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a solution of 13.75 g (0.0967 mole) of 2-fluoro-4-methoxyaniline in 120 mL of toluene was slowly added over a period of 30 minutes a solution of 19.13 g (0.0967 mole) of trichloromethyl chloroformate in 30 mL of toluene. During the addition the temperature rose to 35° C. The reaction mixture was stirred without external heating for 30 minutes and then heated at reflux for approximately 17 hours. At the end of this time all of the solvent was removed by distillation, leaving 2-fluoro-4-methoxyphenyl isocyanate as a purple liquid, which was used immediately in Step D.

후처리

  1. additionDuring the addition the temperature
  2. customrose to 35° C
  3. temperaturewithout external heating for 30 minutes
  4. temperatureheated
  5. temperatureat reflux for approximately 17 hours
  6. customAt the end of this time all of the solvent was removed by distillation

출처 및 근거

ORD 기록
ord-61614fbc8d9a40aaa10bce70a1993c1e
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05262390

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