反应详情

温度

80 °C

0.145 g of 4-tert.-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-6-chloromethyl-2-(morpholin-4-yl)-pyrimidin-4-yl]benzenesulphonamide (Example 4) in 3 ml of acetone was added to a sodium phenolate solution from 0,024 g of phenol and 0.06 g of NaOH in 2 ml of acetone and 1 ml of water. The reaction mixture was stirred at 80° C. under argon for 48 hours. Thereafter, the acetone was distilled off and the residue was partitioned between chloroform and water. The chloroform phase was washed with water, dried over sodium sulphate and the solvent was distilled off. The residue was chromatographed over silica gel with chloroform. 0.07 g of 4-tert.-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-2-morpholin-4-yl-6-phenoxymethyl-pyrimidin-4-yl]benzenesulphonamide, MS: M=639, was obtained.

1. distillationThereafter, the acetone was distilled off
2. customthe residue was partitioned between chloroform and water
3. washThe chloroform phase was washed with water
4. dry with materialdried over sodium sulphate
5. distillationthe solvent was distilled off
6. customThe residue was chromatographed over silica gel with chloroform