반응 #1697988
ord-800a3119fb434fe285993513377a9bc2
반응 방정식
반응 조건
온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1추출the mixture was extracted twice with toluene/ethyl acetate 2/1
- 2건조The combined organic layer was dried (Na2SO4)
- 3여과filtered
- 4기타evaporated
- 5기타The crude product was purified by flash chromatography
실험 절차
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.