반응 #7731

반응 방정식

oxalacetic acid diethyl ester

guanidine carbonate

→

2-Amino-6-oxo-1,6-dihydro-pyrimidine-4-carboxylic acid ethyl ester

용매

water

ethanol

반응 조건

후처리

1. 1
   온도under reflux for 2 hours
2. 2
   농축concentrated
3. 3
   기타to removed ethanol
4. 4
   여과the solid was collected by filtration
5. 5
   온도concentrated hydrochloric acid (1 mL) and refluxed for 15 minutes
6. 6
   온도The mixture was then cooled
7. 7
   workup.ADDITIONdiluted with water
8. 8
   농축concentrated
9. 9
   기타to removed ethanol
10. 10
    여과The white solid was collected by filtration and vacuum
11. 11
    기타dried
12. 12
    기타to give J1.1 (1.67 g, 20%)

실험 절차

A solution of oxalacetic acid diethyl ester (8.5 g, 45.2 mmol) in ethanol (100 mL) was treated with guanidine carbonate (8.1 g, 45.2 mmol) and this was stirred under reflux for 2 hours. The mixture was diluted with water, concentrated to removed ethanol, and the solid was collected by filtration. The solid was then suspended in ethanol (40 mL) and concentrated hydrochloric acid (1 mL) and refluxed for 15 minutes. The mixture was then cooled, basified with potassium carbonate, diluted with water and concentrated to removed ethanol. The white solid was collected by filtration and vacuum dried to give J1.1 (1.67 g, 20%). 1H-NMR (DMSO-d6) δ: 10.34 (1H, br s), 8.92 (1H, br s), 7.46 (1H, br, s), 5.42 (1H, s), 4.18 (2H, q, J=7 Hz), 1.24 (3H, t, J=7 Hz).

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