반응 #581324

반응 방정식

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

methylisocyanate

→

title compound

N-[10-(Benzyloxy)-2-(4-fluorobenzyl)-8-methyl-1,9-dioxo-1,2,6,7,8,9-hexahydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazin-4-yl]-N′-methylurea

용매

1,2-dichloroethane

반응 조건

후처리

1. 1
   농축The product mixture was concentrated under vacuum
2. 2
   workup.DISSOLUTIONThe intermediate dicarbonimidic diamide was dissolved in methanol
3. 3
   workup.ADDITIONtreated with an aqueous solution of KOH (0.1 mL, 2 M)
4. 4
   농축concentrated under vacuum
5. 5
   기타The residue was partitioned between chloroform and dilute hydrochloric acid
6. 6
   추출The organic extract
7. 7
   세척was washed with brine
8. 8
   건조dried over anhydrous magnesium sulfate
9. 9
   여과filtered
10. 10
    농축concentrated under vacuum

실험 절차

A mixture of 4-amino-2-(4-fluorobenzyl)-10-benzyloxy-8-methyl-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione (75 mg, 168 μmol) and methylisocyanate (24 mg, 419 μmol) in anhydrous 1,2-dichloroethane (3 mL) was heated in a sealed tube in an oil bath at 100° C. overnight. The product mixture was concentrated under vacuum. The intermediate dicarbonimidic diamide was dissolved in methanol, treated with an aqueous solution of KOH (0.1 mL, 2 M), and stirred at room temperature for one hour, and concentrated under vacuum. The residue was partitioned between chloroform and dilute hydrochloric acid. The organic extract was washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum to provide the title compound. ES MS M+1=505

출처