反応 #7731

反応方程式

oxalacetic acid diethyl ester

guanidine carbonate

→

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

溶媒

water

ethanol

反応条件

後処理

1. 1
   温度under reflux for 2 hours
2. 2
   濃縮concentrated
3. 3
   その他to removed ethanol
4. 4
   ろ過the solid was collected by filtration
5. 5
   温度concentrated hydrochloric acid (1 mL) and refluxed for 15 minutes
6. 6
   温度The mixture was then cooled
7. 7
   workup.ADDITIONdiluted with water
8. 8
   濃縮concentrated
9. 9
   その他to removed ethanol
10. 10
    ろ過The white solid was collected by filtration and vacuum
11. 11
    その他dried
12. 12
    その他to give J1.1 (1.67 g, 20%)

実験手順

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).

出典