반응 #581306

반응 방정식

ethyl 2-methyl-8-(methoxy)-6-[methoxy(oxo)acetyl]-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine-7-carboxylate

1-methylpiperazin-2-one

N2-Benzyloxycarbonyl-N1-(2,2-dimethoxyethyl)-N1-methylglycinamide

hydrazine acetate

→

title compound

Methyl 10-methoxy-8-methyl-1,9-dioxo-1,2,6,7,8,9-hexahydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-4-carboxylate

용매

acetic acid

반응 조건

후처리

1. 1
   기타prepared in a manner similar to
2. 2
   농축The mixture was concentrated under vacuum
3. 3
   기타The residue was partitioned between chloroform and brine
4. 4
   추출The organic extract
5. 5
   건조was dried over anhydrous magnesium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated under vacuum
8. 8
   기타The residue was triturated in a 4:1 mixture of ethanol and diethyl ether
9. 9
   여과The precipitate was filtered

실험 절차

A solution of ethyl 2-methyl-8-(methoxy)-6-[methoxy(oxo)acetyl]-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine-7-carboxylate (1.28 g, 3.78 mmol; prepared in a manner similar to that described in Example 62, step 5 to 8, starting with 1-methylpiperazin-2-one (Example 7, step 1 to 3) and hydrazine acetate (1.05 g, 11.36 mmol) in glacial acetic acid (8 mL) was heated at 160° C. in an microwave oven for 20 minutes. The mixture was concentrated under vacuum. The residue was partitioned between chloroform and brine. The organic extract was dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residue was triturated in a 4:1 mixture of ethanol and diethyl ether. The precipitate was filtered to afford the title compound. ES MS M+1=321

출처