تفاعل #74007

معادلة التفاعل

3-(2-(2-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)ethoxy)ethoxy)propanoic acid

oxalyl dichloride

→

3-(2-(2-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)ethoxy)ethoxy)propanoyl chloride

المذيبات

DCM

ظروف التفاعل

المعالجة

1. 1
   أخرىInto a 50-mL round-bottom flask purged
2. 2
   درجة الحرارةmaintained with an inert atmosphere of nitrogen
3. 3
   درجة الحرارةThe resulting solution was heated
4. 4
   درجة الحرارةto reflux for 40 min
5. 5
   أخرىThe solvent was removed under vacuum

الإجراء التجريبي

Into a 50-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 3-(2-(2-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)ethoxy)ethoxy)propanoic acid (700 mg, 1.99 mmol, 1.00 equiv) in anhydrous DCM (30.0 mL), then oxalyl dichloride (0.7 mL) was added dropwise at room temperature. Two drops of anhydrous DMF were then added. The resulting solution was heated to reflux for 40 min. The solvent was removed under vacuum to yield 750 mg of 3-(2-(2-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)ethoxy)ethoxy)propanoyl chloride as pale yellow oil, which was used directly for the next reaction step without further purification.

المصدر