反应详情

温度

0 °C

A 1M solution of BBr3 in CH2Cl2 (0.095 ml, 0.095 mmol) was added slowly to a solution of 6-benzyloxy-2-(3,5-dimethylisoxazole-4-sulfonyl)-1-[4-(2-pyrrolidin-1-yl-ethoxy)phenyl]-1,2,3,4-tetrahydroisoquinoline (0.037 g, 0.063 mmol) in anhydrous CH2Cl2 (10 ml) at 0° C. under N2. The reaction mixture was stirred at 0° C. for 1 hr, then warmed to rt and stirred at rt for 4 hr. MeOH (5 ml) was slowly added with stirring and the resulting solution was concentrated in vacuo to an orange residue. Purification by preparative TLC, eluting with EtOAc:MeOH (1:1), and then purification again by preparative TLC, eluting with EtOAc:MeOH (8:2), gave 0.011 g (35% yield) of white solid.

1. temperaturewarmed to rt
2. stirringstirred at rt for 4 hr
3. stirringwith stirring
4. concentrationthe resulting solution was concentrated in vacuo to an orange residue
5. customPurification by preparative TLC
6. washeluting with EtOAc:MeOH (1:1)
7. custompurification again by preparative TLC
8. washeluting with EtOAc:MeOH (8:2)