反応 #518102

反応方程式

Potassium carbonate

2,4-dinitrophenoxyamine

3-[4-cyano-3-methoxyphenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

→

desired product

収率 52.0%

1-Amino-3-[4-cyano-3-methoxyphenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

収率 52.0%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   その他formed
2. 2
   その他were separated off
3. 3
   洗浄washed
4. 4
   洗浄The combined filtrates were washed twice
5. 5
   乾燥dried over sodium sulfate
6. 6
   濃縮concentrated
7. 7
   その他After crystallization

実験手順

Potassium carbonate (1.0 g) and 2,4-dinitrophenoxyamine (0.8 g) were added to a solution of 3-[4-cyano-3-methoxyphenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione (1.1 g) in 15 ml of ethyl acetate. The mixture was subsequently stirred for 15 hours at 55-60° C., whereupon the solids formed were separated off and washed using in each case 30 ml of ethyl acetate and diisopropyl ether. The combined filtrates were washed twice using in each case 25 ml of water, dried over sodium sulfate and then concentrated. After crystallization using 10 ml of diisopropyl ether, 0.6 g of the desired product was obtained. M.p.: >230° C.

出典