Phosgene → Hexan-3-yl carbonochloridate

HRID 328342

Reaktionsgleichung

Reaktionsgleichung von HRID 328342
[CH3:1][CH2:2][CH:3]([OH:7])[CH2:4][CH2:5][CH3:6].[C:8](Cl)([Cl:10])=[O:9]>C1C=CC=CC=1>[Cl:10][C:8]([O:7][CH:3]([CH2:4][CH2:5][CH3:6])[CH2:2][CH3:1])=[O:9]

Komponenten

4

Edukt 2

HCID 6371PhosgeneHCID 121783-Hexanol

Produkt 1

HCID 54555278Hexan-3-yl carbonochloridate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

20.4 G. (0.2 moles) of 3-hexanol is added dropwise under anhydrous conditions to 345 ml. (0.4 moles) of 12.5% phosgene in benzene with stirring and cooling in an ice bath. The addition is complete in 2 hours and 15 minutes and the temperature is allowed to warm to room temperature and the reaction mixture is stirred overnight. Gaseous nitrogen is passed through the solution for several hours to remove the excess phosgene and hydrogen chloride. The reaction mixture is then evaporated to dryness in vacuo affording 28.3 g. (86%) of a colorless oil which infrared analysis indicates to have a strong carbonyl band and no hydroxy band. The oil is used as is in subsequent reactions.

Aufarbeitung

  1. temperaturecooling in an ice bath
  2. additionThe addition
  3. waitGaseous nitrogen is passed through the solution for several hours
  4. customto remove the excess phosgene and hydrogen chloride
  5. customThe reaction mixture is then evaporated to dryness in vacuo
  6. customaffording 28.3 g

Quellen und Nachweise

ORD-Eintrag
ord-8fc70bebe0bd482ba92da717e3671ba9
Quelldatensatz
uspto-grants-1977_04
Patentnummer
US04017505

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