反应详情

A suspension of 5-(2-bromoethyl)benzofurazan (245 mg, 1.08 mmol), 5-(2-methylaminoethoxy)benzofurazan hydrobromide (100 mg, 0.36 mmol), sodium bicarbonate (134 mg, 1.6 mmol) and lithium iodide (2 mg) in ethanol (7.0 ml) was heated at reflux temperature overnight. The reaction mixture was concentrated under reduced pressure and saturated sodium bicarbonate solution added. Extraction with methylene chloride, drying and solvent evaporation gave an oil. Flash chromatography (silica gel, methanol-chloroform, 1%), salt formation and trituration with hexane gave 1-(benzofurazan-5-yl)-2-{N-[2-(benzofurazan-5-oxy)ethyl]-N-methylamino}ethane, hydrochloride (31 mg, 23%); mp 214°-216° C.

1. temperaturewas heated
2. temperatureat reflux temperature overnight
3. concentrationThe reaction mixture was concentrated under reduced pressure and saturated sodium bicarbonate solution
4. additionadded
5. extractionExtraction with methylene chloride
6. customdrying
7. customsolvent evaporation
8. customgave an oil