反应详情

温度

180 °C

A suspension of 2-amino-6-chloro-3-(2,3,5-trichlorophenyl)pyrazine (0.3 g, 9.71×10−4 mole) in absolute ethanol (4 ml) and 0.880 aqueous ammonia (8.24 ml) was stirred and heated in an autoclave at 180° C. for 44 hrs. The cooled mixture was evaporated in vacuo, and the residue extracted with chloroform (3×30 ml). The combined chloroform extracts were dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated down in vacuo. The residue was purified by ‘flash chromatography’ using chloroform to 98:2 chloroform:methanol as the eluent. The product was triturated with 40-60° C. petroleum ether, filtered and dried in vacuo. Yield 0.155 g (56%), M.p. 178-180° C.

1. customThe cooled mixture was evaporated in vacuo
2. extractionthe residue extracted with chloroform (3×30 ml)
3. dry with materialThe combined chloroform extracts were dried over anhydrous magnesium sulphate
4. filtrationfiltered
5. customthe filtrate evaporated down in vacuo
6. customThe residue was purified by ‘flash chromatography’
7. customThe product was triturated with 40-60° C. petroleum ether
8. filtrationfiltered
9. customdried in vacuo