تفاعل #82987

معادلة التفاعل

Trimethyl cyclopropane-1,2,3-tricarboxylate

sodium hydroxide

hydrochloric acid

→

cyclopropane-1,2,3-tricarboxylic acid

المردود 97.0%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheating
2. 2
   درجة الحرارةunder reflux for one hour
3. 3
   درجة الحرارةcooling the reaction product
4. 4
   تركيزconcentrating the reaction solution
5. 5
   workup.ADDITIONadding acetone (200 ml) to the concentrated residue
6. 6
   درجة الحرارةheating the mixture
7. 7
   درجة الحرارةunder reflux for 2 hours
8. 8
   ترشيحfiltering off the precipitate
9. 9
   تركيزconcentrating the filtrate under reduced pressure

الإجراء التجريبي

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%).

المصدر