HRID556653
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
PROCEDURE
实验过程
To a soln of cyclopenteneoxide (2.0 g, 23.8 mmol) in CH3OH and H2O (40 mL) (4/1, v/v), were added NaN3 (7.73 g, 119 mmol) and NH4Cl (3.17 g, 59.2 mmol). The resulting mixture was heated to solvent reflux for 18 h then cooled to 23°. The mixture was concentrated and the residue was diluted with EtOAc, washed with H2O, the organic layer was dried over Na2SO4, concentrated to give the desired product (2.8 g, 93%). 1H NMR (CDCl3): δ 4.10 (m, 1H), 3.72 (m, 1H), 2.10 (m, 2H), 1.72-1.60 (m, 4H).
WORKUP
后处理
- temperatureThe resulting mixture was heated to solvent
- temperaturereflux for 18 h
- temperaturethen cooled to 23°
- concentrationThe mixture was concentrated
- additionthe residue was diluted with EtOAc
- washwashed with H2O
- dry with materialthe organic layer was dried over Na2SO4
- concentrationconcentrated