反应详情

温度

60 °C

0.450 g (1.27 mmole) (3RS)-1-(N-benzyloxycarbonylamidino)-3-mesyloxymethyl pyrrolidine and 0.124 g (1.9 mmole) of sodium azide were dissolved in 10 ml dimethylformamide and heated to 60° C. for four hours followed by stirring at room temperature over night. Water was added and the mixture was extracted twice with toluene/ethyl acetate 2/1. The combined organic layer was dried (Na2SO4), filtered and evaporated. The crude product was purified by flash chromatography using CH2Cl2 /MeOH 95/5 as eluent to yield 0.262 g (68%) of the product.

1. extractionthe mixture was extracted twice with toluene/ethyl acetate 2/1
2. dry with materialThe combined organic layer was dried (Na2SO4)
3. filtrationfiltered
4. customevaporated
5. customThe crude product was purified by flash chromatography