Ethyl orthoformate → HCID 44185486、化合物

HRID 335522ノート

反応式

HRID 335522 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 44185486HCID 44185486、化合物

反応条件

温度
100 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-c929787441fd4ba0a7e3d2a01709e0dc
出典データセット
uspto-grants-2014_11
特許番号
US08884028B2

反応ノート

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