反応 #95385

反応方程式

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

溶媒

dioxane

反応条件

後処理

1. 1
   温度was refluxed for two hours
2. 2
   その他evaporated to dryness in vacuo
3. 3
   workup.DISSOLUTIONThe residue was dissolved in chloroform
4. 4
   洗浄the solution was washed with water
5. 5
   その他dried
6. 6
   その他evaporated to a small volume
7. 7
   その他chromatographed on a 300 gm silicagel column with chloroform and chloroform/methanol (95:5) as the mobile phase
8. 8
   洗浄The 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
    その他the collected hydrochloride was recrystallized from ethanol/water

実験手順

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.

出典