Ethyl orthoformate → HCID 44185486, 화합물

HRID 335522노트

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HRID 335522 반응식
[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]

참가 물질

3

반응물 2

HCID 31214Ethyl orthoformate2회HCID 67697Butanoic acid, 4,4-difluoro-3-oxo-, ethyl ester

생성물 1

HCID 44185486HCID 44185486, 화합물

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온도
100 °C

실험 절차

Process step c): 185.3 g (1.25 mol) of triethyl orthoformate were initially charged in a stirred vessel, the pressure in the vessel was reduced to 500 mbar and the triethyl orthoformate was heated to 100° C. 177.5 g (0.25 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 98° C. to 105° C. within 2 hours. Thereafter, the reaction mixture was stirred at 100° C. for further 3.5 hours. Within this post reaction time the pressure was further reduced to 300 mbar. During the whole reaction time low boiling compounds were removed by distillation under reduced pressure. The resulting suspension (191 g) comprised 16.7% (w/w) of the desired product (GC analysis, quantification with internal standard). The yield, based on ethyl difluoroacetate used, was 57.3%.

후처리

  1. additionwere added at 98° C. to 105° C. within 2 hours
  2. customWithin this post reaction time the pressure
  3. customDuring the whole reaction time low boiling compounds were removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-c929787441fd4ba0a7e3d2a01709e0dc
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08884028B2

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