반응 #570796

반응 방정식

Ethylene glycol

p-toluenesulfonic acid monohydrate

6-chloro-5-formyl-2,3-pyridinedicarboxylic acid, dimethyl ester

toluene

→

title compound

Dimethyl 6-chloro-5-(1,3-dioxolane-2-yl)-2,3-pyridinedicarboxylate

용매

ether

반응 조건

후처리

1. 1
   온도The reaction mixture is heated
2. 2
   온도at reflux temperature for 3 hours
3. 3
   세척washed with saturated sodium bicarbonate solution
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   농축concentrated in vacuo

실험 절차

Ethylene glycol (14.3 mL, 0.255 mol), and a catalytic amount of p-toluenesulfonic acid monohydrate is added to a solution of 6-chloro-5-formyl-2,3-pyridinedicarboxylic acid, dimethyl ester, 5-(dimethyl acetal) (15.46 g, 0.051 mol) and toluene. The reaction mixture is heated at reflux temperature for 3 hours, cooled to room temperature, treated with ether, washed with saturated sodium bicarbonate solution, dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title compound as an orange oil (14.27 g, 93% identified by IR and NMR spectral analyses.

출처