反应详情

After dissolving 10 (8.24 g, 41.9 mmol) into distilled water (60 ml), sodium hydroxide (4.2 g) was added to the solution. After stirring overnight, the solution was neutralized with 1N hydrochloric acid, followed by distillation under a reduced pressure. The residue was dissolved into a mixed solution of water and ethyleneglycoldimethylether (200 ml, 1:1, v/v) to be used for the next reaction. After dissolving sodium hydrogen carbonate (14.1 g) into the solution, 9-fluorenylmethylsuccinimidyl carbonate (16.9 g, 50.1 mmol) was added thereto. After stirring the mixture overnight, precipitates were collected by filtration to obtain 12 (10.8 g, 29.7 mmol). After acidifying the filtrate with 10% hydrochloric acid, precipitates thus generated were collected by filtration and washed with ethyl acetate to further obtain 12 (1.2 g, 3.30 mmol). (Total yield: 12.0 g, 79%)

1. distillationinto distilled water (60 ml), sodium hydroxide (4.2 g)
2. additionwas added to the solution
3. distillationfollowed by distillation under a reduced pressure
4. dissolutionThe residue was dissolved into a mixed solution of water and ethyleneglycoldimethylether (200 ml, 1:1
5. customv/v) to be used for the next reaction
6. additionwas added
7. stirringAfter stirring the mixture overnight
8. customprecipitates
9. filtrationwere collected by filtration