反应详情

184 mg of potassium tert-butoxide are added in three installments, at ambient temperature under argon, to 300 mg of compound of formula (II), 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one, and 170 mg of the compound of formula (III), 2,1,3-benzothiadiazol-5-ylamine, in suspension in 5 ml of DMSO. After a contact time of 30 minutes, the reaction medium is diluted with a mixture of water and ethyl acetate. The aqueous phase is extracted with ethyl acetate and the combined organic phases are then washed with water and then with a saturated NaCl solution. After drying over Na2SO4 and filtering, the solvent is evaporated and then the residue is taken up in a few milliliters of ethyl acetate. The green precipitate obtained is filtered off and then chromatographed on silica (gradient: DCM 100 to DCM/MeOH 90:10). 105 mg of the expected product are isolated in the solid form.

1. extractionThe aqueous phase is extracted with ethyl acetate
2. washthe combined organic phases are then washed with water
3. dry with materialAfter drying over Na2SO4
4. filtrationfiltering
5. customthe solvent is evaporated
6. customThe green precipitate obtained
7. filtrationis filtered off
8. customchromatographed on silica (gradient: DCM 100 to DCM/MeOH 90:10)