反应详情

To 1-4 (27.9 g, 0.082 moles) dissolved in DMSO (400 ml) was added sodium azide (5.61 g, 0.086 moles) at room temperature and the resulting solution was heated at 65° for 2 hrs. The cooled reaction mixture was diluted with 250 ml EtOAc, extracted with 2×100 ml portions of water, 2×50 ml portions of brine and then dried (MgSO4). Solvent removal provided 1-5 as a pale yellow oil, Rf 0.5 (silica gel, 20% acetone/hexane). ##STR13##

1. temperaturethe resulting solution was heated at 65° for 2 hrs
2. customThe cooled reaction mixture
3. extractionextracted with 2×100 ml portions of water, 2×50 ml portions of brine
4. dry with materialdried (MgSO4)
5. customSolvent removal