Реакция #74007

Уравнение реакции

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

Растворители

DCM

Условия реакции

Обработка

1. 1
   ДругоеInto a 50-mL round-bottom flask purged
2. 2
   Температураmaintained with an inert atmosphere of nitrogen
3. 3
   ТемператураThe resulting solution was heated
4. 4
   Температураto reflux for 40 min
5. 5
   ДругоеThe solvent was removed under vacuum

Методика

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.

Источник