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

HRID 899557노트

반응식

HRID 899557 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 2723922Sodium ethoxide용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3ffb696f2b594d4ab30b29ce2e614fb7
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07355065B2

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