反应详情

1 g of 4,6-dichloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)-pyrimidine and 1.43 g of 5-isopropyl pyridine-2-sulfonamide potassium salt were suspended in 20 ml of dry DMF. The mixture was stirred under argon at room temperature and became clear within a few h. After 16 h at room temperature, most of the solvent was removed by evaporation under reduced pressure. The residue was taken up in 20 ml water and the pH was adjusted to 4-5 by adding about 1 ml of acetic acid. A precipitate formed. The precipitate was filtered off, washed with water and dried. The yellow powder was further purified by column chromatography on silica gel eluting first with hexane:ethyl acetate 1:1 then with DCM:MeOH 10:1. 1.43 g of 5-isopropyl-N-[6-chloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)-4-pyrimidinyl]-2-pyridine sulfonamide was obtained as a slightly yellow powder. LC-MS: tR=5.00 min, [M+1]+=512.19, [M−1]−=510.26.

1. custommost of the solvent was removed by evaporation under reduced pressure
2. additionby adding about 1 ml of acetic acid
3. customA precipitate formed
4. filtrationThe precipitate was filtered off
5. washwashed with water
6. customdried
7. customThe yellow powder was further purified by column chromatography on silica gel eluting first with hexane:ethyl acetate 1:1