Reaktion #63166

ord-5acd77535c4a4c6691f2c1b53feccebc

Reaktionsgleichung

O=C(Cl)Cl
phosgene
O=C(Cl)Cl
phosgene
Cl
hydrogen chloride
O=C1CCCCCO1
6-caprolactone
Cl
hydrogen chloride
C[N+]1(C)CCCCC1.[Cl-]
N,N-dimethylpiperidinium chloride
O=C(Cl)CCCCCCl
6-chlorohexanoyl chloride
O=C1CCCCCO1
caprolactone

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeare passed in at 170°-175° C. in the course of 7 hours
  2. 2
    workup.WAITThe reaction mixture is then kept at this temperature for a further hour
  3. 3
    workup.DISTILLATIONthe reaction mixture is then worked up by distillation under reduced pressure

Vorschrift

456 parts of 6-caprolactone and 9 parts of N,N-dimethylpiperidinium chloride are initially taken in the stirred reactor described in Example 1. 380 parts of phosgene and 70 parts of hydrogen chloride are passed in at 170°-175° C. in the course of 7 hours. The reaction mixture is then kept at this temperature for a further hour. Any phosgene and hydrogen chloride still present are blown out with nitrogen, and the reaction mixture is then worked up by distillation under reduced pressure. 424 parts of 6-chlorohexanoyl chloride and 86 parts of caprolactone are obtained. The conversion is 81% and the yield is 77.3%, based on lactone used.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04764309uspto-grants-1988_08