反应详情

A solution of 4,6-dichloro-5-(2-methoxyphenoxy)-2-(4-pyridyl)-pyrimidine (1.75 g, Referential Example 7) and 2-pyridin-2-yl-ethanesulfonic acid amide potassium salt (1.13 g) in DMSO (30 ml) was stirred at rt for 24 h. Triethylamine (657 mg) was added and stirring was continued for another 96 h before the mixture was diluted with ethyl acetate (150 ml) and washed 4% aq. citric acid and water. The aqueous phase was extracted three more times with EA. The organic phase was dried over MgSO4 and evaporated. The crude product was purified by column chromatography on silica gel eluting with EA containing 0–10% methanol to give 2-pyridin-2-yl-ethanesulfonic acid [6-chloro-5-(2-methoxyphenoxy)-2-pyridin-4-yl-pyrimidin-4-yl]-amide (950 mg) as a brown powder. LC-MS: tR=3.63 min, [M+1]+=498.31, [M−1]−=496.10.

1. washwashed 4% aq. citric acid and water
2. extractionThe aqueous phase was extracted three more times with EA
3. dry with materialThe organic phase was dried over MgSO4
4. customevaporated
5. customThe crude product was purified by column chromatography on silica gel eluting with EA containing 0–10% methanol