反应详情

To a solution of Compound 4 (1.9 g, 9.3 mmol) in DMF (35 mL), 2-succinimido-1,1,3,3-tetramethyluronium tetrafluoroborate (3.4 g, 11.2 mmol) and N,N-diisopropyl ethylamine (3.4 mL, 19.5 mmol) were added. Combined mixture was stirred at room temperature for 30 mins and then a solution of 2-amino-5-diethylaminopentane (2.2 g, 13.9 mmol) in DMF (5 mL) was added. After stirring the mixture for additional 1 hour, it was poured in brine (100 mL) and extracted with ethyl acetate (2×75 mL). The combined organic layers were washed with brine (3×100 mL) and dried over MgSO4. The solvent was removed under reduced pressure to provide Compound 5 as a dark yellow viscous liquid (2.64 g, 82.5%). This product was used without further purification. The structure of Compound 5 is given below:

1. stirringAfter stirring the mixture for additional 1 hour
2. extractionextracted with ethyl acetate (2×75 mL)
3. washThe combined organic layers were washed with brine (3×100 mL)
4. dry with materialdried over MgSO4
5. customThe solvent was removed under reduced pressure