反应详情

温度

90 °C

A mixture of the isothiourea dihydrochloride from Example 1 (i) (8.3 g), hydrazine sulphate (4.1 g), potassium hydrogen carbonate (12.5 g) and anhydrous dimethyl formamide (100 ml) was stirred at 90° C. for 3 hours. Following cooling and filtration from inorganic material, the filtrate containing the free base was treated with ethanolic hydrogen chloride. The residue was then triturated with isopropanol to give a solid which was recrystallised from aqueous isopropanol to give the title compound (1.94 g), m.p. 234°-235°.

1. temperatureFollowing cooling
2. filtrationfiltration from inorganic material
3. additionthe filtrate containing the free base
4. additionwas treated with ethanolic hydrogen chloride
5. customThe residue was then triturated with isopropanol
6. customto give a solid which
7. customwas recrystallised from aqueous isopropanol