반응 #216538

반응 방정식

2,4,6-triiodophenol

2-propylvaleroyl chloride

sodium bicarbonate

→

pure product

수율 68.0%

2,4,6-Triiodophenyl (2-propyl)pentanoate

수율 68.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도was refluxed under argon overnite
2. 2
   온도The reaction mixture was cooled
3. 3
   추출extracted with dichloromethane
4. 4
   추출The dichloromethane extract
5. 5
   건조was dried over magnesium sulfate
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   기타to give the crude product (2.42 mmol, 95%) as a pink solid
9. 9
   기타Recrystallization from ethyl acetate

실험 절차

A mixture of 2,4,6-triiodophenol (2.0 g, 4.24 mmol), 2-propylvaleroyl chloride (2.5 ml, 12.7 mmol, 3 eq) and 4-dimethylaminopyridine (DMAP; 20 mg) in 20 ml of acetonitrile was refluxed under argon overnite. The reaction mixture was cooled and poured into excess aqueous sodium bicarbonate and then extracted with dichloromethane. The dichloromethane extract was dried over magnesium sulfate, filtered, and evaporated to give the crude product (2.42 mmol, 95%) as a pink solid. Recrystallization from ethyl acetate gave 1.75 g (68%) of pure product, mp 99°-101° C.

출처