2,3-Pyridinedicarboxylic anhydride synthesis
- Product Name:2,3-Pyridinedicarboxylic anhydride
- CAS Number:699-98-9
- Molecular formula:C7H3NO3
- Molecular Weight:149.1
89-00-9
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699-98-9
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Yield:699-98-9 91%
Reaction Conditions:
with oxalyl dichloride;N,N-dimethyl-formamide in toluene for 3 h;Inert atmosphere;Reflux;
Steps:
General procedure for the preparation of cyclic anhydrides 1a-v
General procedure: Dicarboxylic acid 2 (1 mmol) and oxalyl chloride (1.2 mmol) were combined in dry toluene (5 mL) and a drop of freshly distilled DMF was added. The reaction vessel was purged with argon and the reaction was heated under stirring for 3 h. The stirring was stopped and the toluene solution was decanted off the oily residue and filtered. Evaporation of the volatiles provided the analytically pure target product which, if necessary, was transformed intro crystalline form by trituration with diethyl ether. In some cases (see ESI) additional crystallization or trituration with 1:2 v/v hexane-toluene mixture was used. .
References:
Kantin, Grigory;Chupakhin, Evgeny;Dar'in, Dmitry;Krasavin, Mikhail [Tetrahedron Letters,2017,vol. 58,# 32,p. 3160 - 3163] Location in patent:supporting information
