反応 #94198

反応方程式

ethyl bromopyruvate

4-methylquinazoline

ethyl bromopyruvate

→

product

2-Carbethoxypyrrolo[1,2-c]quinazoline

溶媒

ethanol

反応条件

後処理

1. 1
   温度at reflux for two hours
2. 2
   その他During this time, a tan solid formed
3. 3
   温度to reflux overnight
4. 4
   その他The alcohol was removed in vacuo
5. 5
   workup.ADDITIONthe residue diluted with H2O
6. 6
   workup.ADDITIONSodium bicarbonate was added until effervescence
7. 7
   抽出the aqueous mixture extracted with ether
8. 8
   乾燥dried over Na2SO4
9. 9
   ろ過filtered
10. 10
    その他the solvent removed in vacuo
11. 11
    その他to yield a tan solid
12. 12
    その他Crystallization from MeOH

実験手順

A solution of ethyl bromopyruvate (3.2g, 0.016 m) and 4-methylquinazoline (2.0g, 0.014 m) in dry ethanol (150 ml) was heated at reflux for two hours. During this time, a tan solid formed. Excess ethyl bromopyruvate was added (1.0g) and the reaction mixture was allowed to reflux overnight. After this time, the reaction was complete. The alcohol was removed in vacuo and the residue diluted with H2O. Sodium bicarbonate was added until effervescence ceased and the aqueous mixture extracted with ether. The ether extracts were combined, dried over Na2SO4, filtered and the solvent removed in vacuo to yield a tan solid. Crystallization from MeOH afforded the product as a white solid; m.p. 138°-139° C.

出典