Reaktion #1581729

Reaktionsgleichung

dimethyl 5-dimethoxymethylpyridine-2,3-dicarboxylate

→

title compound

Ausbeute 84.2%

DIMETHYL 5-FORMYLPYRIDINE-2,3-DICARBOXYLATE

Ausbeute 84.2%

Lösungsmittel

HCl

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux temperature for 2 hours
2. 2
   SonstigeThe tetrahydrofuran is removed in vacuo
3. 3
   workup.ADDITIONthe aqueous solution is diluted with water (to 30 mL)
4. 4
   Extraktionextracted with methylene chloride
5. 5
   TrocknenThe combined methylene chloride extracts are dried over anhydrous magnesium sulfate
6. 6
   Einengenconcentrated in vacuo

Vorschrift

A solution of dimethyl 5-dimethoxymethylpyridine-2,3-dicarboxylate (6.57 g, 0.024 mol) in 2N HCl (15 mL) and tetrahydrofuran (25 mL) is stirred at reflux temperature for 2 hours. The tetrahydrofuran is removed in vacuo, the aqueous solution is diluted with water (to 30 mL) and extracted with methylene chloride. The combined methylene chloride extracts are dried over anhydrous magnesium sulfate and concentrated in vacuo to yield the title compound (4.51 g, 82%) as a yellow solid, mp 75°-77° C., identified by IR and NMR spectral analyses.

Quelle