反应详情

0.2 g of [2-(3-ethyl-5-methyl-2-oxo-1,3,5-triazinan-1-yl)-6-nitro-1,3-benzothiazol-7-yl]methyl cyanide was charged into about 2 ml dimethylformamide. About 15 equivalents of triethylamine were then added followed by about 15 equivalents of trimethylsilyl chloride. The solution was stirred at room temperature for about 4–20 hours. The reaction was quenched by pouring into dilute aqueous hydrochloric acid then extracted well with ethyl acetate. The combined organics were back extracted with dilute sodium bicarbonate then dried over magnesium sulfate and concentrated. The dark oil was further purified by preparative HPLC to yield 2-(3-ethyl-5-methyl-2-oxo-1,3,5-triazinan-1-yl) [1,3]thiazolo[5′,4′: 3,4]benzo[c]isoxazol-8-yl cyanide.

1. customThe reaction was quenched
2. additionby pouring into dilute aqueous hydrochloric acid
3. extractionthen extracted well with ethyl acetate
4. extractionThe combined organics were back extracted with dilute sodium bicarbonate
5. dry with materialthen dried over magnesium sulfate
6. concentrationconcentrated
7. customThe dark oil was further purified by preparative HPLC