HRID2101522

反应详情

EQUATION

反应方程式

HRID 2101522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-[1-(3,5-Dichloro-benzyl)-1H-imidazol-2-ylmethoxy]-phenylamine (see Example 21) in CH2Cl2 and phenyl isocyanate in CH2Cl2 (0.4 mL) were combined and the reaction was shaken at room temperature. After 72 h, LC/MS showed the reaction had progressed to completion. Trisamine resin was added and the reaction was shaken at room temperature. After 4 h, the reaction was filtered and the resin was washed with CH2Cl2 (2 mL). The filtrates were combined and concentrated in vacuo. Preparatory TLC (silica, 20:1 CH2Cl2:MeOH; Rf=0.5) yielded 1-{3-[1-(3,5-dichloro-benzyl)-1H-imidazol-2-ylmethoxy]-phenyl}-3-phenyl-urea (25a) as a white solid (22 mg, 52%); MS m/z 467 [C24H20Cl2N4O2+H]+.

WORKUP

后处理

  1. stirringthe reaction was shaken at room temperature
  2. waitAfter 4 h
  3. filtrationthe reaction was filtered
  4. washthe resin was washed with CH2Cl2 (2 mL)
  5. concentrationconcentrated in vacuo