反应详情

A mixture of N-(1-ethylpyrazol-5-yl)-5-(methylthio) anthranilic acid (4.5 g) and POCl3 (20 ml) is refluxed overnight. The reaction mixture is poured into water, then ice is added. The mixture is extracted with CH2Cl2 and then the CH2Cl2 layer is evaporated. The residue is purified by column chromatography on silica gel eluting with 50% ethyl acetate/hexane to afford 2.4 g of 1-ethyl-4-chloro-6-(methylthio)-1H-pyrazolo[3,4-b]quinoline, m.p. 120°-121° C.

1. temperatureis refluxed overnight
2. additionice is added
3. extractionThe mixture is extracted with CH2Cl2
4. customthe CH2Cl2 layer is evaporated
5. customThe residue is purified by column chromatography on silica gel eluting with 50% ethyl acetate/hexane