Diphosgene → 4-Chloro-2-fluorophenyl isocyanate

HRID 846525

反応式

HRID 846525 の反応式
[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

参加物

4

反応物 2

HCID 10426DiphosgeneHCID 938984-Chloro-2-fluoroaniline

生成物 1

HCID 45582034-Chloro-2-fluorophenyl isocyanate収率 97.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8100e6eb8a6942ee91490dd4284198b3
出典データセット
uspto-grants-1992_08
特許番号
US05136868

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