Diphosgene → 4-Chloro-2,3-dihydro-2,2-dimethylbenzofuran-7-yl isocyanate

HRID 440654노트

반응식

HRID 440654 반응식
[NH2:1][C:2]1[C:10]2[O:9][C:8]([CH3:12])([CH3:11])[CH2:7][C:6]=2[C:5]([Cl:13])=[CH:4][CH:3]=1.Cl[C:15](OC(Cl)(Cl)Cl)=[O:16]>C1(C)C=CC=CC=1>[Cl:13][C:5]1[C:6]2[CH2:7][C:8]([CH3:11])([CH3:12])[O:9][C:10]=2[C:2]([N:1]=[C:15]=[O:16])=[CH:3][CH:4]=1

참가 물질

4

반응물 2

HCID 10426DiphosgeneHCID 224047737-Amino-4-chloro-2,3-dihydro-2,2-dimethylbenzofuran

생성물 1

HCID 153462864-Chloro-2,3-dihydro-2,2-dimethylbenzofuran-7-yl isocyanate수율 99.7%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution of 1.97 g (0.010 mole) of 7-amino-4-chloro-2,3-dihydro-2,2-dimethylbenzofuran in 60 mL of toluene was added slowly 1.2 mL (0.010 mole) of trichloromethyl chloroformate. This mixture was stirred at ambient temperature for one hour and then was heated at reflux for approximately 16 hours. At the conclusion of this period the solvent was evaporated from the reaction mixture under reduced pressure, leaving 2.23 g of 4-chloro-2,3-dihydro-2,2-dimethylbenzofuran-7-yl isocyanate as an oil.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for approximately 16 hours
  3. customAt the conclusion of this period the solvent was evaporated from the reaction mixture under reduced pressure

출처 및 근거

ORD 기록
ord-89ed21e2b5e043df8fc9252b13124aa5
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521147

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