HRID386889

反应详情

EQUATION

反应方程式

HRID 386889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 933.0 mg (2.74 mmol) of {3-[1,1-dimethyl-2-(tetrahydro-pyran-2-yloxy)-ethyl]-isoxazol-5-yl}-carbamic acid tert-butyl ester and 103.0 mg (0.41 mmol) of pyridinium p-toluenesulfonate in ethanol (8.0 mL) is stirred at 65° C. for 1 h. After this time, the reaction mixture is concentrated under reduced pressure. Purification by flash chromatography on silica gel using ethyl acetate/heptane provides 602.0 mg of the title compound. Yield: 85.7%. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 1.3 (6H, s), 1.55 (9H, s), 2.35 (1H, t, J=8.0 Hz), 3.7 (2H, d, J=8.0 Hz), 6.5 (1H, s), 7.3 (1H, s).

WORKUP

后处理

  1. concentrationAfter this time, the reaction mixture is concentrated under reduced pressure
  2. customPurification by flash chromatography on silica gel