反应详情

To a of 0° C. cooled solution of 1.00 g (2.10 mmol) (7R,8R,9R)-10-acetyl-7-(2-methoxyethoxy)-2-methyl-9-phenyl-8-pivaloyloxy-7.8.9.10-tetrahydroimidazo[1.2-h][1.7]naphthyridine in ethanol (20 ml) is added 0.28 g (2.10 mmol) NCS and the mixture is stirred for 2 h. Afterwards the reaction is quenched by adding of saturated aqueous sodium hydrogen carbonate solution and is extracted twice with dichloromethane. The combined organic layers are washed with brine, dried over sodium sulphate and evaporated in vacuo. The crude product is purified by column chromatography (ethyl acetate/cylohexane: 1/1) to provide 0.89 g (1.73 mmol/82%) of the title compound as a colourless solid with a melting point of 167–170° C. (cyclohexane).

1. customAfterwards the reaction is quenched
2. additionby adding of saturated aqueous sodium hydrogen carbonate solution
3. extractionis extracted twice with dichloromethane
4. washThe combined organic layers are washed with brine
5. dry with materialdried over sodium sulphate
6. customevaporated in vacuo
7. customThe crude product is purified by column chromatography (ethyl acetate/cylohexane: 1/1)