HRID2101498

反应详情

EQUATION

反应方程式

HRID 2101498 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 [1-(3,5-dichloro-benzyl)-1H-imidazol-2-ylmethyl]-(3-fluoro-benzyl)-(2-piperazin-1-yl-ethyl)-amine (55 mg, 0.12 mmol) in CH2Cl2 at ambient temperature was added dropwise Ac2O (34 μL, 0.36 mmol). The mixture was stirred for 2 h before addition of saturated NaHCO3 (6 mL). The mixture was extracted with CH2Cl2 (2×20 mL) and the combined extracts dried over Na2SO4 then concentrated in vacuo. The residue was purified by semi-preparative HPLC to provide the title compound (42 mg, 66%) as a viscous oil: ESI MS m/z 518 [C26H30Cl2FN5O+H]+.

WORKUP

后处理

  1. extractionThe mixture was extracted with CH2Cl2 (2×20 mL)
  2. dry with materialthe combined extracts dried over Na2SO4
  3. concentrationthen concentrated in vacuo
  4. customThe residue was purified by semi-preparative HPLC