HRID2249845

反应详情

EQUATION

反应方程式

HRID 2249845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureThe resulting mixture was heated to solvent
  2. temperaturereflux for 18 h
  3. temperaturethen cooled to 23°
  4. concentrationThe mixture was concentrated
  5. additionthe residue was diluted with EtOAc
  6. washwashed with H2O
  7. dry with materialthe organic layer was dried over Na2SO4
  8. concentrationconcentrated