تفاعل #438675

معادلة التفاعل

(1,3-dioxolan-4-yl)methyl 5-norbornene-2-carboxylate

glycerol formal

methyl 5-norbornene-2-carboxylate

sodium methoxide

→

1,3-dioxan-5-yl 5-norbornene-2-carboxylate

المردود 93.0%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةunder reflux for 5 hours
3. 3
   workup.DISTILLATIONwhile gradually distilling off methanol
4. 4
   أخرىformed during the reaction
5. 5
   درجة الحرارةAfter cooling
6. 6
   غسيلthe reaction solution was washed with saturated sodium bicarbonate water
7. 7
   تجفيفdried over anhydrous sodium sulfate
8. 8
   تركيزconcentrated in vacuum
9. 9
   workup.DISTILLATIONIt was further purified by vacuum distillation

الإجراء التجريبي

A mixture of 104 g of glycerol formal, 152 g of methyl 5-norbornene-2-carboxylate, 2.0 g of sodium methoxide and 300 ml of toluene was heated under reflux for 5 hours while gradually distilling off methanol formed during the reaction. After cooling, the reaction solution was washed with saturated sodium bicarbonate water, dried over anhydrous sodium sulfate, and concentrated in vacuum. It was further purified by vacuum distillation, obtaining 209 g of a mixture of (1,3-dioxolan-4-yl)methyl 5-norbornene-2-carboxylate and 1,3-dioxan-5-yl 5-norbornene-2-carboxylate (boiling point 111-115° C./530 Pa, yield 93%).

المصدر