반응 #6430

반응 방정식

methyl succinimidyl adipate

chlorotrimethylsilane

sodium iodide

→

adipic acid monosuccinimidyl ester

수율 75.2%

용매

acetonitrile

ethyl acetate

반응 조건

후처리

1. 1
   온도at reflux for 12 hours
2. 2
   세척The reaction mixture was washed repeatedly with 5 percent aqueous sodium bisulfite until the organic solution
3. 3
   세척Then it was washed with brine
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated

실험 절차

A solution of methyl succinimidyl adipate (4.5 g, 17.5 mmol), chlorotrimethylsilane (11.1 ml, 87.5 mmol) and sodium iodide (13.1 g, 87.5 mmol) in 10 ml of acetonitrile was heated at reflux for 12 hours. The mixture was then cooled to room temperature and diluted with ethyl acetate. The reaction mixture was washed repeatedly with 5 percent aqueous sodium bisulfite until the organic solution was colorless. Then it was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated to provide 3.2 g (71 percent yield by weight) of adipic acid monosuccinimidyl ester as a white solid.

출처