HRID1678659

反应详情

EQUATION

反应方程式

HRID 1678659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 2-[2-(4-chloro-phenyl)-2H-indazol-3-yl]-2-cyclohexyl-ethanol (20 mg, 56 umol) in THF (1 ml) was added 4-hydroxy-3,5-dimethyl-benzoic acid methyl ester (11 mg, 62 umol; CAS Reg. No. 34137-14-9) and tri-phenylphosphine (18 mg, 68 umol) at ambient temperature under an argon atmosphere. The mixture was cooled to 0° C., di-tert-butyl azodicarboxylate (16 mg, 68 umol) was added and the suspension was stirred for 14 h at ambient temperature. The solvent was removed under reduced pressure to give a solid which was purified by column chromatography (silica gel, iPrOAc/heptane) to obtain the title compound (8 mg, 15 umol; 27%) as colorless oil. MS: m/e=517.3 [M+H+].

WORKUP

后处理

  1. customat ambient temperature
  2. customThe solvent was removed under reduced pressure
  3. customto give a solid which
  4. customwas purified by column chromatography (silica gel, iPrOAc/heptane)