Ethyl orthoformate → HCID 44185486、化合物

HRID 335523ノート

反応式

HRID 335523 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
105 °C

実験手順

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.

後処理

  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%

出典と根拠

ORDレコード
ord-68f46da9da33473abc1dd8d5a5227533
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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