反应详情

A mixture of 0.614 g of compound of formula (II), 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one, and 0.389 g of the compound of formula (III), (1,3-dihydro-5-isobenzofuranyl)amine, is heated in 10 ml of acetic acid at reflux for 20 min; the reaction medium is concentrated by half under vacuum, then taken up in a mixture of ethyl acetate and water and brought to pH 9 with a saturated NaHCO3 solution. After separating by settling, the organic phase is washed with water and then with a saturated NaCl solution, dried over sodium sulfate and then evaporated to dryness. The product is purified by flash chromatography on silica with a gradient of 0 to 50% of ethyl acetate in dichloromethane. 0.140 g of expected product is obtained in the form of a yellow solid.

1. temperatureat reflux for 20 min
2. concentrationthe reaction medium is concentrated by half under vacuum
3. additiontaken up in a mixture of ethyl acetate and water
4. customAfter separating
5. washthe organic phase is washed with water
6. dry with materialwith a saturated NaCl solution, dried over sodium sulfate
7. customevaporated to dryness
8. customThe product is purified by flash chromatography on silica with a gradient of 0 to 50% of ethyl acetate in dichloromethane