반응 #956
ord-d3631dc5ac684ec9b01dd5b9b7ce5987
반응 방정식
1-benzyloxycarbonylamidino-4-mesyloxyethyl piperidine
sodium azide
water
→
4-Azidoethyl-1-benzyloxycarbonylamidino piperidine
반응 조건
온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.ADDITIONwas added
- 2추출extracted with ethyl acetate three times
- 3세척The combined organic phase was washed with water
- 4건조dried (Na2SO4)
- 5기타evaporated
- 6기타chromatographed on silica gel
실험 절차
In 100 ml of dimethylformamide was dissolve (0.0115 mol) of crude 1-benzyloxycarbonylamidino-4-mesyloxyethyl piperidine and 4.5 g (0.069 mol) of sodium azide was added. The mixture was heated at 100° C. for 2.5 h. It was then poured into water and extracted with ethyl acetate three times. The combined organic phase was washed with water, dried (Na2SO4) and evaporated. The residue was flash chromatographed on silica gel using ethyl acetate/heptane 1/1 as eluent. Yield: 3.0 g (79%).