反应详情

1.2 gm of chloroacetyl chloride were added to a stirred solution of 2.2 gm of 2,6-diamino-benzo[1,2-d:5,4-d']bisthiazole in 20 ml of dimethylformamide at 5° C. The resulting suspension was heated for 1 hour on a waterbath, then cooled, and the solid 2,6-bis-(chloroacetyl-amino)-benzo[1,2-d:5,4-d']bisthiazole was filtered off. While stirring, 0.5 gm of an aqueous saturated sodium carbonate solution was added to the filtrate. After 1 hour the precipitate was filtered off, dissolved in 30 ml of dimethylformamide/dioxan (1:1), freed from traces of insoluble material and precipitated again with water. The crystals were dissolved in dimethylformamide and the solution was treated with an excess of 2 N hydrochloric acid. The hydrochloride obtained thereby was washed and dried.

1. temperatureThe resulting suspension was heated for 1 hour on a waterbath
2. temperaturecooled
3. filtrationthe solid 2,6-bis-(chloroacetyl-amino)-benzo[1,2-d:5,4-d']bisthiazole was filtered off
4. addition0.5 gm of an aqueous saturated sodium carbonate solution was added to the filtrate
5. filtrationAfter 1 hour the precipitate was filtered off
6. dissolutiondissolved in 30 ml of dimethylformamide/dioxan (1:1)
7. customprecipitated again with water
8. dissolutionThe crystals were dissolved in dimethylformamide
9. additionthe solution was treated with an excess of 2 N hydrochloric acid