HRID1040447
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
To a round bottom flask was added (1-cyano-cyclopropyl)-carbamic acid benzyl ester (500 mg, 2.31 mmol) in DMF (4 ml), followed by the addition of NaN3 (195 mg, 3 mmol) and NH4Cl (161 mg, 3 mmol). The reaction mixture was stirred at 110° C. for 24 h. The reaction mixture was concentrated in vacuo. The residue was dissolved in EtOAc/water. The organic layer was separated, washed with brine, dried under any. Na2SO4, filtered and concentrated to afford 380 mg of [1-(1H-tetrazol-5-yl)-cyclopropyl]-carbamic acid benzyl ester as a off-white solid, m/z 260.8 [M+1]+.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- dissolutionThe residue was dissolved in EtOAc/water
- customThe organic layer was separated
- washwashed with brine
- customdried under any
- filtrationNa2SO4, filtered
- concentrationconcentrated