反应详情

A mixture of N-(1-ethylpyrazol-5-yl)-5-bromoanthranilic acid (12.6 g) and POCl3 (30 ml) is refluxed overnight. The reaction mixture is poured into ice water (500 ml), stirred for 20 minutes, and then NH4OH is added until a pH of 8-10 is obtained. The mixture is stirred for 0.5 hours, and then the solid that forms is collected by filtration. The solid is dissolved in CH2Cl2, dried over MgSO4 and purified by column chromatography on silica gel eluting with 30% hexane/ethyl acetate to afford 6.5 g of 1-ethyl-4-chloro-6-bromo-1H-pyrazolo[3,4-b]quinoline, m.p. 117°-118° C.

1. temperatureis refluxed overnight
2. customis obtained
3. stirringThe mixture is stirred for 0.5 hours
4. filtrationthe solid that forms is collected by filtration
5. dissolutionThe solid is dissolved in CH2Cl2
6. dry with materialdried over MgSO4
7. custompurified by column chromatography on silica gel eluting with 30% hexane/ethyl acetate