Hydrochloric Acid → Cyclopropane-1,2,3-tricarboxylic acid

HRID 54709노트

반응식

HRID 54709 반응식
[CH:1]1([C:12]([O:14]C)=[O:13])[CH:3]([C:4]([O:6]C)=[O:5])[CH:2]1[C:8]([O:10]C)=[O:9].[OH-].[Na+].Cl>CO>[CH:2]1([C:8]([OH:10])=[O:9])[CH:3]([C:4]([OH:6])=[O:5])[CH:1]1[C:12]([OH:14])=[O:13]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12659895Trimethyl cyclopropane-1,2,3-tricarboxylate

생성물 1

HCID 699248Cyclopropane-1,2,3-tricarboxylic acid수율 97%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Trimethyl cyclopropane-1,2,3-tricarboxylate (20.6 g, 95.2 mmols) was dissolved in methanol (200 ml), followed by dropwise adding sodium hydroxide (23.7 g, 593 mmol) (dissolved in water (100 ml)) at room temperature, thereafter heating and reacting the mixture under reflux for one hour, cooling the reaction product, adding conc. hydrochloric acid (40 g, 1.1 mol), concentrating the reaction solution, adding acetone (200 ml) to the concentrated residue, heating the mixture under reflux for 2 hours, filtering off the precipitate, and concentrating the filtrate under reduced pressure, to obtain cyclopropane-1,2,3-tricarboxylic acid (16.0 g, 91.9 mmol, 97%).

후처리

  1. temperatureheating
  2. temperatureunder reflux for one hour
  3. temperaturecooling the reaction product
  4. concentrationconcentrating the reaction solution
  5. additionadding acetone (200 ml) to the concentrated residue
  6. temperatureheating the mixture
  7. temperatureunder reflux for 2 hours
  8. filtrationfiltering off the precipitate
  9. concentrationconcentrating the filtrate under reduced pressure

출처 및 근거

ORD 기록
ord-c5fe50e6123044209265219794a0709b
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05623078

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