HRID1689774

反应详情

EQUATION

反应方程式

HRID 1689774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-[5-cyclopropyl-3-(2,6-dichloro-phenyl)-isoxazol-4-ylmethoxy]-azepane-1-carboxylic acid tert-butyl ester (2.0 g, 0.00416 mol) in CH2Cl2 (20 ml) is added trifluoroacetic acid (1.42 g, 0.01248 mol) at 0° C. under N2 atmosphere. Stir the mixture for 3 h at room temperature. Concentrate the reaction mixture in vacuo to give crude product. Purify by column chromatography over alumina (neutral) eluting with 8:2 dichloromethane/methanol to give the title compound 1.4 g (88%). ES/MS m/z 381.1 (M+1).

WORKUP

后处理

  1. concentrationConcentrate the reaction mixture in vacuo
  2. customto give crude product
  3. customPurify by column chromatography over alumina (neutral)
  4. washeluting with 8:2 dichloromethane/methanol