Ethyl orthoformate → HCID 44185486, Verbindung

HRID 335523Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 335523
[CH:1]([O:8][CH2:9][CH3:10])([O:5]CC)OCC.[F:11][CH:12]([F:21])[C:13](=[O:20])[CH2:14][C:15]([O:17][CH2:18][CH3:19])=O>>[CH2:9]([O:8][C:1](=[O:5])/[C:14](=[CH:15]\[O:17][CH2:18][CH3:19])/[C:13](=[O:20])[CH:12]([F:21])[F:11])[CH3:10]

Komponenten

3

Edukt 2

HCID 31214Ethyl orthoformate2×HCID 67697Butanoic acid, 4,4-difluoro-3-oxo-, ethyl ester

Produkt 1

HCID 44185486HCID 44185486, Verbindung

Reaktionsbedingungen

Temperatur
105 °C

Versuchsvorschrift

Process step c): 778.1 g (5.25 mol) of triethyl orthoformate were charged in a stirred vessel, the pressure within the vessel was slowly reduced to 310 mbar and the triethyl orthoformate was heated to 104° C. 121.1 g (0.175 mol-100% conversion in process steps a) and b) assumed) of ethyl 4,4-difluoroacetoacetate (in the form of a suspension coming from process step b)) were added at 103° C. to 104° C. within 2 hours. Thereafter, the reaction mixture was stirred at 105° C. for further 30 minutes. During the entire reaction time low boiling compounds were removed by distillation under reduced pressure. Afterwards, the suspension was cooled down to room temperature. The resulting suspension (761 g) comprised 4.36% (w/w) of the desired product (GC analysis, quantification with internal standard). This corresponds to an overall yield over the two synthetic steps of 85.4%, based on ethyl difluoroacetate used.

Aufarbeitung

  1. additionwere added at 103° C. to 104° C. within 2 hours
  2. customDuring the entire reaction time low boiling compounds were removed by distillation under reduced pressure
  3. temperatureAfterwards, the suspension was cooled down to room temperature
  4. customThis corresponds to an overall yield over the two synthetic steps of 85.4%

Quellen und Nachweise

ORD-Eintrag
ord-68f46da9da33473abc1dd8d5a5227533
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08884028B2

Notizen zur Reaktion

Wird geladen…