Hydrochloric Acid → Butanoic acid, 4,4-difluoro-3-oxo-, ethyl ester

HRID 899557ノート

反応式

HRID 899557 の反応式
C(N(CC)[C:4](=[O:8])[CH:5]([F:7])[F:6])C.Cl.[C:12]([O:15][CH2:16][CH3:17])(=[O:14])[CH3:13]>[O-]CC.[Na+]>[CH2:16]([O:15][C:12](=[O:14])[CH2:13][C:4](=[O:8])[CH:5]([F:6])[F:7])[CH3:17]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 12557633N,N-Diethyl-2,2-difluoroacetamide

生成物 1

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

試薬・触媒・溶媒 1

HCID 2723922Sodium ethoxide溶媒

反応条件

温度
60 °C

実験手順

In a sulfonation flask, N,N-diethyl-2,2-difluoroacetamide (1.51 g; 10 mmol) was dissolved in ethyl acetate (20 ml) before ethanolic sodium ethoxide (15 ml of a 21% solution; 40.2 mmol) was added dropwise. The resulting mixture was stirred at 60° C. for 6 hours. After cooling, the mixture was poured into ice-water (20 ml), acidified with hydrochloric acid (10%) and extracted with ethyl acetate. The organic phase was washed with brine, dried over sodium sulfate and evaporated in a water jet vacuum. The residue was purified by distillation under reduced pressure to give the desired 4,4-difluoro-3-oxo-butanoic acid ethyl ester in the form of a colourless oil.

後処理

  1. addition40.2 mmol) was added dropwise
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was washed with brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated in a water jet vacuum
  7. distillationThe residue was purified by distillation under reduced pressure

出典と根拠

ORDレコード
ord-3ffb696f2b594d4ab30b29ce2e614fb7
出典データセット
uspto-grants-2008_04
特許番号
US07355065B2

反応ノート

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