反应详情

A mixture of the isothiourea trihydrochloride from Example 2 (ii) (5.1 g), methoxyamine hydrochloride (2.5 g), potassium hydrogen carbonate (5.0 g) and water (30 ml) was refluxed for 24 hours. The products were partitioned between N sodium hydroxide and n-butanol. The n-butanol solution was then extracted with N hydrochloric acid, and the extracts concentrated and dissolved in isopropanol. After filtration from inorganic material, the filtrate gave the title compound (0.6 g). When a solution in aqueous ethanol of this compound was eluted from an ion exchange column of IRA-401 in nitrate form, the corresponding trinitrate was obtained.

1. temperaturewas refluxed for 24 hours
2. customThe products were partitioned between N sodium hydroxide and n-butanol
3. extractionThe n-butanol solution was then extracted with N hydrochloric acid
4. concentrationthe extracts concentrated
5. dissolutiondissolved in isopropanol
6. filtrationAfter filtration from inorganic material