HRID413434

反应详情

EQUATION

反应方程式

HRID 413434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[1-Amino-4-[2-(3-hydroxy-phenyl)-ethylamino]-1-(3-methyl-3H-imidazol-4-yl)-butyl]-2-fluoro-benzonitrile (0.058 g, 0.142 mmol) was dissolved in DMF (15 mL) and treated with Cs2CO3 (0.324 g, 0.994 mmol). After 18 h at 60° C., the reaction mixture was concentrated in vacuo, dissolved in H2O: 0.1% TFA (3 mL) and purified by RP LC on a Delta PrepPak eluting with 95:5 to 5:95 H2O (0.1% TFA): CH3CN(0.1% TFA) to give the title compound as an 80:20 mixture of enantiomers.

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. dissolutiondissolved in H2O
  3. custom0.1% TFA (3 mL) and purified by RP LC on a Delta PrepPak
  4. washeluting with 95:5 to 5:95 H2O (0.1% TFA)