反应详情

In a 100 ml, round-bottom flask equipped with a stir bar, 6-[4-(4-Benzyl-phthalazin-1-yl)-piperazin-1-yl]-nicotinonitrile (150 mg, 0.362 mmol) is dissolved in anhydrous EtOH (7 mL) followed by the addition of NiCl2 (0.398 mmol). NaBH4 (0.723 mmol) is added in portions and the reaction is stirred for 2 h under a N2 atmosphere. The septum is removed and Ac2O (1.08 mmol) is added. The reaction is capped again and stirred for one additional hour. LC/MS shows full conversion to the acylated product. The reaction is filtered through a Celite pad and rinsed with 50 ml of MeOH. The final compound is purified by preparative HPLC using a C-18 column and propanol as the modifier (85 mg, 52% yield).

1. customIn a 100 ml, round-bottom flask equipped with a stir bar
2. customThe septum is removed
3. customThe reaction is capped again
4. stirringstirred for one additional hour
5. filtrationThe reaction is filtered through a Celite pad
6. washrinsed with 50 ml of MeOH
7. customThe final compound is purified by preparative HPLC