反応 #6984

反応方程式

methyl-3-(methoxycarbonyl)amino-4-methoxy-isoxazole-5-carboxylate

sodium hydroxide

hydrochloric acid

→

white solid

3-(methoxycarbonyl)amino-4-methoxy-isoxazole-5-carboxylic acid

溶媒

water

反応条件

後処理

1. 1
   その他prepared
2. 2
   温度After cooling
3. 3
   その他to exceed 5° C
4. 4
   その他the precipitate obtained
5. 5
   ろ過is filtered off
6. 6
   洗浄washed with cold water

実験手順

A mixture of 2.50 g (0.011 mmol) of methyl-3-(methoxycarbonyl)amino-4-methoxy-isoxazole-5-carboxylate (prepared according to the method described in W. Kloetzer, J. Schantz, Monatsh. Chem., 1965, 102–115) and 1.30 g of powdered sodium hydroxide dissolved in 9 ml of water is heated at 90° C. for 3 hours. After cooling, the mixture is acidified to pH=2 with concentrated hydrochloric acid, controlling the temperature so as not to exceed 5° C. After 1 hour of stirring at 0° C., the precipitate obtained is filtered off and washed with cold water. There is obtained 2.01 g (86% yield) of a white solid (M+1=217).

出典