Ethyl Propionate → Ethyl 2-Formylpropionate

HRID 128615

반응식

HRID 128615 반응식
[CH:1]([O:3][CH2:4][CH3:5])=[O:2].[C:6](OCC)(=[O:9])[CH2:7][CH3:8].[H-].[Na+].[H][H]>C1COCC1.O>[CH:6]([CH:7]([CH3:8])[C:1]([O:3][CH2:4][CH3:5])=[O:2])=[O:9]

참가 물질

7

반응물 4

HCID 7749Ethyl PropionateHCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 10898741Ethyl 2-Formylpropionate

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of ethyl formate (55.2 g) and ethyl propionate (51.0 g) was added dropwise with stirring to a suspension of sodium hydride (20.9 g, 60% dispersion in mineral oil) in dry THF (260 ml) under nitrogen. On completion of the addition, the temperature of the reaction mixture rose gradually from ambient temperature to 45° C. accompanied by rapid evolution of hydrogen. The reaction mixture was stirred for 2 hours then cooled and water (400 ml) was added cautiously. The basic solution was washed with ether, then acidified with dilute hydrochloric acid and extracted with ether to give an oil. The oil was distilled and the fraction boiling in the range 100°-160° C. was collected to give ethyl 2-formylpropionate.

후처리

  1. additionwas added dropwise
  2. additionOn completion of the addition
  3. customrose gradually from ambient temperature to 45° C.
  4. temperaturethen cooled
  5. washThe basic solution was washed with ether
  6. extractionextracted with ether
  7. customto give an oil
  8. distillationThe oil was distilled
  9. customboiling in the range 100°-160° C.
  10. customwas collected

출처 및 근거

ORD 기록
ord-409d15a94f9c4de7be13f878054718bf
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05464781

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