反应详情

Oxalyl chloride (5.71 g, 45 mmol., 3.0 eq) was added dropwise, at ambient temperature, to a solution of 4-isopropyl-thiazole-2-carboxylic acid (3.85 g, 22.5 mmol., 1.5 eq) in toluene (40 mL). Stirring was continued at ambient temperature until the bubbling stopped. The reaction mixture was then heated under reflux for a further 1 hour. LCMS analysis of an aliquot quenched with methanol revealed full conversion of the acid to the acid chloride. The reaction mixture was left to cool to ambient temperature and the solvent removed under vacuum. The crude material was used directly in the next step without further purification.

1. customwas continued at ambient temperature until the bubbling
2. temperatureThe reaction mixture was then heated
3. temperatureunder reflux for a further 1 hour
4. customLCMS analysis of an aliquot quenched with methanol revealed full conversion of the acid to the acid chloride
5. waitThe reaction mixture was left
6. customthe solvent removed under vacuum
7. customThe crude material was used directly in the next step without further purification