반응 #640621

반응 방정식

Oxalyl chloride

4-isopropyl-thiazole-2-carboxylic acid

→

4-isopropylthiazole-2-carbonyl chloride

용매

toluene

반응 조건

후처리

1. 1
   기타was continued at ambient temperature until the bubbling
2. 2
   온도The reaction mixture was then heated
3. 3
   온도under reflux for a further 1 hour
4. 4
   기타LCMS analysis of an aliquot quenched with methanol revealed full conversion of the acid to the acid chloride
5. 5
   workup.WAITThe reaction mixture was left
6. 6
   기타the solvent removed under vacuum
7. 7
   기타The crude material was used directly in the next step without further purification

실험 절차

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.

출처