反应详情

温度

0 °C

A mixture of 1-amino-2-[3-(3-piperidinomethylphenoxy)-propylamino]-1-cyclobutene-3,4-dione [prepared in Step A] (2.68 g, 0.0078 mole), 2-propanol (8.5 mL), and 1M aqueous hydrochloric acid (8.0 mL, 0.008 mole) was heated to reflux with stirring. Insoluble material was removed by filtration and acetone (24 mL) was added to the hot solution. The mixture was stirred at ambient temperature for 18 hours, then cooled to 0° C. The solid was collected by filtration, washed with acetone:2-propanol (2:1) (3 mL), and dried in vacuo to give 1.67 g (56.4% yield) of the title compound as an off-white powder. The product was shown by spectral data to be identical to authentic sample of the hydrochloride salt.

1. temperaturewas heated
2. temperatureto reflux
3. customInsoluble material was removed by filtration and acetone (24 mL)
4. additionwas added to the hot solution
5. stirringThe mixture was stirred at ambient temperature for 18 hours
6. filtrationThe solid was collected by filtration
7. washwashed with acetone:2-propanol (2:1) (3 mL)
8. customdried in vacuo