Sodium Hydroxide → 1-(Ethoxycarbonyl)cyclopropanecarboxylic acid

HRID 35268

반응식

HRID 35268 반응식
[OH-].[Na+].[C:3]1([C:11]([O:13]CC)=[O:12])([C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:5][CH2:4]1>O.C(O)C>[CH2:9]([O:8][C:6]([C:3]1([C:11]([OH:13])=[O:12])[CH2:4][CH2:5]1)=[O:7])[CH3:10]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 73790Diethyl cyclopropane-1,1-dicarboxylate

생성물 1

HCID 117894721-(Ethoxycarbonyl)cyclopropanecarboxylic acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of sodium hydroxide (2.15 g, 54 mmol) in water (15 ml) was added dropwise to a stirred solution of diethyl 1,1-cyclopropanedicarboxylate (10 g, 54 mmol) in ethanol (30 ml) while the temperature was maintained below 25° C. After the completion of the addition, the resulting mixture was stirred at room temperature for 60 hours. Most of ethanol was removed by evaporation in vacuo and the residue was diluted with brine, acidified with 6N hydrochloric acid and extracted with diethyl ether. The extract was dried over magnesium sulfate, filtered and concentrated. The residue was purified by distillation to give the title compound (bp 66°-9° C./0.15 mm) as a viscous oil.

후처리

  1. temperaturewas maintained below 25° C
  2. additionAfter the completion of the addition
  3. customMost of ethanol was removed by evaporation in vacuo
  4. additionthe residue was diluted with brine
  5. extractionextracted with diethyl ether
  6. dry with materialThe extract was dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. distillationThe residue was purified by distillation

출처 및 근거

ORD 기록
ord-956c15967e91447aac7dce6276966152
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766145

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