Phosgene → 2-Ethylbutyl carbonochloridate

HRID 328343

Reaktionsgleichung

Reaktionsgleichung von HRID 328343
[CH2:1]([CH:3]([CH2:6][CH3:7])[CH2:4][OH:5])[CH3:2].[C:8](Cl)([Cl:10])=[O:9].ClC([O-])=O>C1C=CC=CC=1>[Cl:10][C:8]([O:5][CH2:4][CH:3]([CH2:6][CH3:7])[CH2:1][CH3:2])=[O:9]

Komponenten

5

Edukt 3

HCID 6371PhosgeneHCID 73582-Ethyl-1-butanolHCID 21226386Carbonochloridate

Produkt 1

HCID 544120422-Ethylbutyl carbonochloridate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

20.4 G. (0.2 moles) of 2-ethyl-1-butanol is added dropwise under anhydrous conditions to 250 ml. (0.4 moles) of 17.2% phosgene solution in benzene with stirring in an ice bath. The addition is complete in 70 minutes and the solution is allowed to gradually warm to room temperature and stirred for 16 hours. The excess phosgene and hydrogen chloride are removed with a stream of nitrogen and the residual solution evaporated to dryness in vacuo affording 17.9 g. (54%) of a light yellow oil which IR demonstrates having a strong chloroformate band and no hydroxy. The oil is used as is in further reactions.

Aufarbeitung

  1. additionThe addition
  2. customThe excess phosgene and hydrogen chloride are removed with a stream of nitrogen
  3. customthe residual solution evaporated to dryness in vacuo
  4. customaffording 17.9 g

Quellen und Nachweise

ORD-Eintrag
ord-efbfbebf66014f23bbf37360e380f506
Quelldatensatz
uspto-grants-1977_04
Patentnummer
US04017505

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