反应详情

温度

60 °C

2-amino-5-hydroxy-benzoic acid (15 mmol) are suspended in ethanol (water free, 600 ml) and heated up to 60° C. and stirred. Then triethylamine (30 mmol) is added and a clear solution is formed. Ethoxy-imino-acetic acid ethyl ester (16.5 mmol) is added at 60° C. and after 15 minutes another portion of triethylamine (15 mmol) is added and the mixture stirred for another 30 minutes. The mixture is cooled down to RT and left at RT without stirring over night. The solid material formed was filtered off, washed with ethanol/ether and dried (vacuum). A pale brown powder with mp. 258-260° C. (decomposition) is obtained.

1. customa clear solution is formed
2. additionis added
3. stirringthe mixture stirred for another 30 minutes
4. temperatureThe mixture is cooled down to RT
5. waitleft at RT
6. stirringwithout stirring over night
7. customThe solid material formed
8. filtrationwas filtered off
9. washwashed with ethanol/ether
10. customdried (vacuum)
11. customA pale brown powder with mp. 258-260° C. (decomposition) is obtained