HRID1422649

反应详情

EQUATION

反应方程式

HRID 1422649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of methyl 3-hydroxy-5-methyl-3-phenylhex-5-enyl(2-methylbut-3-yn-2-yl)carbamate (26 mg, 0.081 mmol) and azidobenzene (29 mg, 0.24 mmol) in H2O (1 mL) and t-BuOH (1 mL) was added ascorbic acid (3.2 mg, 0.016 mmol)followed by CuSO4.H2O (0.5 mg, 0.002 mmol). The mixture was stirred at rt for 2 d. Additional azidobenzene (29 mg, 0.24 mmol), ascorbic acid (3.2 mg, 0.016 mmol) and CuSO4.5H2O (0.5 mg, 0.002 mmol) were added. The mixture was stirred for 4 h at rt and purified by prep HPLC to afford methyl 3-hydroxy-5-methyl-3-phenylhex-5-enyl(2-(1-phenyl-1H-1,2,3-triazol-4-yl)propan-2-yl)carbamate (16 mg, 44%) as an oil. LC-MS Method 1 tR=2.00 min, m/z=449.

WORKUP

后处理

  1. stirringThe mixture was stirred for 4 h at rt
  2. custompurified by prep HPLC