反应详情

The reaction was effected as described in Example 61, but using a solution of 1.5 mmol of 2-[5-(1,2-dithiolan-3-yl)pentyl]isoindole-1,3-dione in 3 ml of toluene, 2 ml of methanol, 2 ml of butylamine, 4 ml of pyridine and 230 mg of succinic anhydride. The solvent was removed from the reaction mixture by distillation under reduced pressure. Water was added to the residue, after which it was extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and then dried over anhydrous sodium sulfate. Ethyl acetate was removed from the extract by distillation under reduced pressure and the residue was subjected to reverse phase preparative silica gel column chromatography, using 2:3, 1:1 and 3:2 by volume mixtures of acetonitrile and water as eluent. Acetonitrile was removed from the eluate so obtained by distillation under reduced pressure. The residue was extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and then dried over anhydrous sodium sulfate. Ethyl acetate was removed from the extract by distillation under reduced pressure. The residue was dissolved in dioxane, after which it was lyophilised, to give 166 mg of the title compound as a pale yellow amorphous substance, melting at 74° C.

1. customThe solvent was removed from the reaction mixture by distillation under reduced pressure
2. additionWater was added to the residue
3. extractionafter which it was extracted with ethyl acetate
4. washThe extract was washed with a saturated aqueous solution of sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. customEthyl acetate was removed from the
7. extractionextract by distillation under reduced pressure
8. customAcetonitrile was removed from the eluate
9. customso obtained by distillation under reduced pressure
10. extractionThe residue was extracted with ethyl acetate
11. washThe extract was washed with a saturated aqueous solution of sodium chloride
12. dry with materialdried over anhydrous sodium sulfate
13. customEthyl acetate was removed from the
14. extractionextract by distillation under reduced pressure
15. dissolutionThe residue was dissolved in dioxane