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

HRID 440654Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 440654
[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

Komponenten

4

Edukt 2

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

Produkt 1

HCID 153462864-Chloro-2,3-dihydro-2,2-dimethylbenzofuran-7-yl isocyanateAusbeute 99,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-89ed21e2b5e043df8fc9252b13124aa5
Quelldatensatz
uspto-grants-1996_05
Patentnummer
US05521147

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