تفاعل #95385

معادلة التفاعل

2,6-bis-(chloroacetyl-amino)-benzo[1,2-d:5,4-d']bisthiazole

di-n-propylamine

→

2,6-Bis-(di-n-propylamino-acetylamino)-benzo[1,2-d:5,4-d']bisthiazole dihydrochloride

المذيبات

dioxane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed for two hours
2. 2
   أخرىevaporated to dryness in vacuo
3. 3
   workup.DISSOLUTIONThe residue was dissolved in chloroform
4. 4
   غسيلthe solution was washed with water
5. 5
   أخرىdried
6. 6
   أخرىevaporated to a small volume
7. 7
   أخرىchromatographed on a 300 gm silicagel column with chloroform and chloroform/methanol (95:5) as the mobile phase
8. 8
   غسيلThe title compound, 2.5 gm (25.5% of theory), was eluted
9. 9
   workup.DISSOLUTIONdissolved in chloroform
10. 10
    workup.ADDITIONtreated with gaseous hydrogen chloride
11. 11
    أخرىthe collected hydrochloride was recrystallized from ethanol/water

الإجراء التجريبي

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.

المصدر