反应详情

温度

50 °C

To a solution of (R)-(+)-2-bromo-α-methylbenzyl alcohol (402 mg, 2.0 mmol) and diphenylphosphoryl azide (0.692 ml, 3.2 mmol) in THF (10 mL) was added 1,8-diazabicyclo[5.4.0]undec-7-ene (0.466 ml, 3.2 mmol). The mixture was heated at 50° C. for overnight, partitioned with H2O and AcOEt, and then adjusted to pH 7 by adding 1M HCl. The organic layer was dried with MgSO4, filtered and evaporated. The residue was purified by silica gel column chromatography [eluting with n-hexane/AcOEt=95/5] to give the title compound (381 mg, 84%).

1. custompartitioned with H2O and AcOEt
2. additionby adding 1M HCl
3. dry with materialThe organic layer was dried with MgSO4
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by silica gel column chromatography [eluting with n-hexane/AcOEt=95/5]