methyl 3-[5-(dithiolan-3-yl)pentanoylamino]propanoate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The reaction was effected as described in Example 49, but using 213 mg of methyl 3-[5-(1,2-dithiolan-3-yl)pentanoylamino]propionate (prepared as described in Example 55), 4 ml of methanol and 1.80 ml of a 1N aqueous solution of sodium hydroxide. The solvent was removed from the reaction mixture by distillation under reduced pressure. Water was added to the residue. The resulting mixture was neutralized by the addition of 2N aqueous hydrochloric acid, 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. The residue was dissolved in dioxane, after which it was lyophilised, to give 0.11 g of the title compound as a pale yellow amorphous substance, melting at 74 to 76° C. The solvent was removed from the reaction mixture by distillation under reduced pressure Water was added to the residue The resulting mixture was neutralized by the addition of 2N aqueous hydrochloric acid after which it was extracted with ethyl acetate The extract was washed with a saturated aqueous solution of sodium chloride dried over anhydrous sodium sulfate Ethyl acetate was removed from the extract by distillation under reduced pressure The residue was dissolved in dioxane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The reaction was effected as described in Example 49, but using 213 mg of methyl 3-[5-(1,2-dithiolan-3-yl)pentanoylamino]propionate (prepared as described in Example 55), 4 ml of methanol and 1.80 ml of a 1N aqueous solution of sodium hydroxide. The solvent was removed from the reaction mixture by distillation under reduced pressure. Water was added to the residue. The resulting mixture was neutralized by the addition of 2N aqueous hydrochloric acid, 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. The residue was dissolved in dioxane, after which it was lyophilised, to give 0.11 g of the title compound as a pale yellow amorphous substance, melting at 74 to 76° C. The solvent was removed from the reaction mixture by distillation under reduced pressure Water was added to the residue The resulting mixture was neutralized by the addition of 2N aqueous hydrochloric acid after which it was extracted with ethyl acetate The extract was washed with a saturated aqueous solution of sodium chloride dried over anhydrous sodium sulfate Ethyl acetate was removed from the extract by distillation under reduced pressure The residue was dissolved in dioxane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The reaction was effected as described in Example 49, but using 213 mg of methyl 3-[5-(1,2-dithiolan-3-yl)pentanoylamino]propionate (prepared as described in Example 55), 4 ml of methanol and 1.80 ml of a 1N aqueous solution of sodium hydroxide. The solvent was removed from the reaction mixture by distillation under reduced pressure. Water was added to the residue. The resulting mixture was neutralized by the addition of 2N aqueous hydrochloric acid, 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. The residue was dissolved in dioxane, after which it was lyophilised, to give 0.11 g of the title compound as a pale yellow amorphous substance, melting at 74 to 76° C. The solvent was removed from the reaction mixture by distillation under reduced pressure Water was added to the residue The resulting mixture was neutralized by the addition of 2N aqueous hydrochloric acid after which it was extracted with ethyl acetate The extract was washed with a saturated aqueous solution of sodium chloride dried over anhydrous sodium sulfate Ethyl acetate was removed from the extract by distillation under reduced pressure The residue was dissolved in dioxane