反应详情

温度

0 °C

To a of 0° C. cooled solution of 10.5 g (35.8 mmol) (8R,9R)-8-hydroxy-2-methyl-9-phenyl-7,8,9,10-tetrahydroimidazo[1,2-h][1,7]naphthyridin-7-one in dichloromethane (110 ml) is added 5.70 ml (41.2 mmol) triethylamine, 0.22 g (1.80 mmol) dimethylaminopyridine and 5.10 ml (41.2 mmol) pivaloyl chloride dissolved in dichloromethane (10 ml). The reaction is stirred for 2 h at 0° C. and warmed up to 25° C. and stirred for further 24 h. Afterwards 5.70 ml (41.2 mmol) triethylamine, 0.22 9 (1.80 mmol) dimethylaminopyridine and 5.10 ml (41.2 mmol) pivaloyl chloride are added to this mixture and it is stirred for 18 h at 25° C. Subsequently the reaction is quenching by adding of water (100 ml). The organic layer is separated, washed with ammonia solution, washed with water two times, dried over sodium sulphate and evaporated in vacuo. The crude product is crystallised from 2-propanol to provide 12.1 g (32.06 mmol/90%) of the title compound as a colourless solid with a melting point of 145-147° C. (2-propanol).

1. temperaturewarmed up to 25° C.
2. stirringstirred for further 24 h
3. stirringis stirred for 18 h at 25° C
4. customSubsequently the reaction is quenching
5. additionby adding of water (100 ml)
6. customThe organic layer is separated
7. washwashed with ammonia solution
8. washwashed with water two times
9. dry with materialdried over sodium sulphate
10. customevaporated in vacuo
11. customThe crude product is crystallised from 2-propanol