反应详情

A mixture of 7.2 gm of 2,6-bis-(chloroacetyl-amino)-benzo[1,2-d:5,4-d']bisthiazole, 10 gm of di-n-propylamine and 100 ml of dioxane was refluxed for two hours and then evaporated to dryness in vacuo. The residue was dissolved in chloroform, and the solution was washed with water, dried, evaporated to a small volume and chromatographed on a 300 gm silicagel column with chloroform and chloroform/methanol (95:5) as the mobile phase. The title compound, 2.5 gm (25.5% of theory), was eluted, dissolved in chloroform, treated with gaseous hydrogen chloride, and the collected hydrochloride was recrystallized from ethanol/water. M.P. 210° C.

1. temperaturewas refluxed for two hours
2. customevaporated to dryness in vacuo
3. dissolutionThe residue was dissolved in chloroform
4. washthe solution was washed with water
5. customdried
6. customevaporated to a small volume
7. customchromatographed on a 300 gm silicagel column with chloroform and chloroform/methanol (95:5) as the mobile phase
8. washThe title compound, 2.5 gm (25.5% of theory), was eluted
9. dissolutiondissolved in chloroform
10. additiontreated with gaseous hydrogen chloride
11. customthe collected hydrochloride was recrystallized from ethanol/water