反应详情

温度

75 °C

A solution of 50 mg of 2-picolinic acid azide (prepared from 2-picolinic acid according to Chem. Pharm. Bull. 25 (1977) 1651-1657) and 10 mg of DMAP in 8 ml of chloroform was stirred for 1 h at 75° C. 50 mg of 5-isopropyl-N-[6-(4-hydroxy-2-butynyloxy)-5-(o-methoxyphenoxy)-2-(4-pyridyl)-4-pyrimidinyl]-2-pyridine sulfonamide (Example 1g) followed by 3 ml of DMF was added and the resulting clear solution was stirred for 16 h at 75° C. The mixture was diluted with 75 ml of ethyl acetate and washed with 50 ml of 10% aqueous citric acid followed by 50 ml of water. The organic layer was evaporated and the crude product was purified by chromatography on prep. tlc-plates with dichlormethane:methanol 10:1 to give 41 mg of 2-pyridinyl-carbamic acid 4-[6-(5-isopropyl-pyridine-2-sulfonylamino)-5-(2-methoxy-phenoxy)-2-pyridin-4-yl-pyrimidin-4-yloxy]-but-2-ynyl ester as a white solid. LC-MS: tR=4.74 min, [M+1]+=682.47, [M−1]−=680.41.

1. additionwas added
2. washwashed with 50 ml of 10% aqueous citric acid
3. customThe organic layer was evaporated
4. customthe crude product was purified by chromatography on prep