반응 #581329

반응 방정식

10-(benzyloxy)-4-bromo-2-(4-fluorobenzyl)-8-methyl-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

1-methylpiperazin-2-one

→

title compound

2-(4-Fluorobenzyl)-10-hydroxy-8-methyl-4-(4-methyl-3-oxopiperazin-1-yl)-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

반응 조건

후처리

1. 1
   기타phase preparative HPLC purification
2. 2
   기타Collection and lyophilization of appropriate fractions

실험 절차

A mixture of 10-(benzyloxy)-4-bromo-2-(4-fluorobenzyl)-8-methyl-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione (0.10 g, 0.19 mmol; Example 160, Step 1) and 1-methylpiperazin-2-one (2 mL) was heated in a sealed tube in an oil bath at 100° C. overnight. The benzyl protecting group was also cleaved in the process. The reaction mixture was subjected to reverse phase preparative HPLC purification. Collection and lyophilization of appropriate fractions provided the title compound.

출처