反应详情

To a solution of 139 (0.173 g, 0.773 mmol) and DCM (5 mL) at RT was added TEA (0.235 g, 2.32 mmol) and CDI (0.125 g, 0.773 mmol) and the reaction was stirred at RT for 30 min. To this solution was added dropwise a solution of 216 (0.200 g, 0.773 mmol), TEA (0.235 g, 2.32 mmol) and DCM (5 mL) and the resulting solution stirred for 4 h then poured into water and extracted with DCM. The combined organic fractions were dried (MgSO4), filtered, and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with DCM/MeOH (500:40) to afford 0.050 g (14.8%) of I-57: MS m/z (APCI-pos) M+1=436.

1. stirringthe resulting solution stirred for 4 h
2. extractionextracted with DCM
3. dry with materialThe combined organic fractions were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by SiO2 chromatography
7. washeluting with DCM/MeOH (500:40)
8. customto afford 0.050 g (14.8%) of I-57: MS m/z (APCI-pos) M+1=436