反应详情

A solution of 1.4 g. 2,2-dimethyl-3-nitroxypropanoyl chloride in 50 ml. dry tetrahydrofuran is added dropwise at ambient temperature to a solution of 2.3 g. 3-(2-amino-1,1-dimethylethylamino)-1-(3-methylbenzimidazol-4-yloxy)-propan-2-ol in 150 ml. dry tetrahydrofuran, followed by further stirring for 2 hours. The reaction mixture is evaporated and chromatographed on silica gel with methylene chloride/methanol (4:2 v/v). The product obtained (2.0 g.) is dissolved in 60 ml. methylene chloride and mixed with 0.54 g. fumaric acid in 100 ml. acetone. The precipitate which separates out after the addition of 200 ml. diethyl ether is filtered off with suction and dried. There are obtained 2.3 g. (53% of theory) of the desired product in the form of crystals; m.p. 187°-190° C.

1. customThe reaction mixture is evaporated
2. customchromatographed on silica gel with methylene chloride/methanol (4:2 v/v)
3. customThe product obtained (2.0 g.)
4. dissolutionis dissolved in 60 ml
5. additionafter the addition of 200 ml
6. filtrationdiethyl ether is filtered off with suction
7. customdried
8. customThere are obtained 2.3 g