反应详情

温度

0 °C

A round bottomed flask cooled to 0° C., was charged 7-(benzylthio)-4-chloro-2-(4-methoxybenzyl)isoquinolin-1(2H)-one (0.400 g, 0.948 mmol), DCM (9.03 ml), Acetic Acid (0.226 ml), and Water (0.226 ml). After stirring for 5 minutes at 0° C., sulfuryl chloride (0.077 ml, 0.948 mmol) was added and stirring was continued for an additional 1 hour at 0° C. The reaction was concentrated, dissolved in minimal DCM and purified via column chromatography (silica gel 40 g, gradient elution 0 to 50% EtOAc:Heptane) to afford 0.342 g of 4-chloro-2-(4-methoxybenzyl)-1-oxo-1,2-dihydroisoquinoline-7-sulfonyl chloride. m/z (ESI) 399.2 (M+H)+.

1. stirringstirring
2. waitwas continued for an additional 1 hour at 0° C
3. concentrationThe reaction was concentrated
4. dissolutiondissolved in minimal DCM
5. custompurified via column chromatography (silica gel 40 g, gradient elution 0 to 50% EtOAc:Heptane)