反应详情

A solution of 4-(6-chloropyrimidine-4-carboxamido)-3-methylbenzene-1-sulfonyl chloride (Intermediate 30, 1.2g; 3.47 mmol) in THF (100 ml) was treated with methyl 2-(methylamino)acetate (666 mg; 4.77 mmol) and diisopropylamine (2 ml; 14.3 mmol). After stirring at RT for 18 hours the solvent was removed in vacuo and the residue redissolved in DCM and washed with water. The organic extracts were passed through a hydrophobic frit and the solvent removed in vacuo. The residue was purified by column chromatography (silica) eluting with petroleum ether containing increasing amounts of EtOAc. The title product was obtained as a white solid.

1. customwas removed in vacuo
2. dissolutionthe residue redissolved in DCM
3. washwashed with water
4. customthe solvent removed in vacuo
5. customThe residue was purified by column chromatography (silica)
6. washeluting with petroleum ether containing
7. temperatureincreasing amounts of EtOAc