Diphosgene → 4-Chloro-2-fluorophenyl isocyanate

HRID 846525

반응식

HRID 846525 반응식
[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([F:9])[CH:3]=1.Cl[C:11](OC(Cl)(Cl)Cl)=[O:12]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([N:6]=[C:11]=[O:12])=[C:4]([F:9])[CH:3]=1

참가 물질

4

반응물 2

HCID 10426DiphosgeneHCID 938984-Chloro-2-fluoroaniline

생성물 1

HCID 45582034-Chloro-2-fluorophenyl isocyanate수율 97.7%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a stirred solution of 20.0 grams (0.13 mole) of 4-chloro-2-fluoroaniline in 250 ml of toluene was added dropwise a solution of 17.2 ml (0.13 mole) of trichloromethyl chloroformate in 40 ml of toluene. Upon completion of addition the reaction mixture was heated to reflux where it stirred for 16 hours. The solvent was separated from the reaction mixture by distillation to yield 21.8 grams of 4-chloro-2-fluorophenyl isocyanate as an oil. The reaction was repeated several times.

후처리

  1. additionUpon completion of addition the reaction mixture
  2. temperaturewas heated
  3. temperatureto reflux where it
  4. customThe solvent was separated from the reaction mixture by distillation

출처 및 근거

ORD 기록
ord-8100e6eb8a6942ee91490dd4284198b3
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05136868

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