HRID62073

反应详情

EQUATION

反应方程式

HRID 62073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 3-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)propan-1-amine (1 equiv) and sodium bicarbonate (5 equiv) in an appropriate reaction vessel may be added a solvent such as dichloromethane (at a concentration between about 0.01 M to about 1 M). The reaction may be placed in an ice bath and triphosgene (0.4 equiv) can be added in one portion. The reaction may be monitored by LC/MS to observe formation of the isocyanate, upon which the reaction may be diluted with dichloromethane, filtered through a phase separator, and concentrated. The residue may be suspended in a solvent such as acetonitrile (0.1 M to about 1 M), followed by addition of 3,5-dimethylaniline (1.0-1.5 equiv) and cesium carbonate (1.0-1.5 equiv). Following completion of the reaction, the product may be obtained using standard organic chemistry techniques of workup and purification.

WORKUP

后处理

  1. concentrationat a concentration between about 0.01 M to about 1 M)
  2. customThe reaction
  3. custommay be placed in an ice bath
  4. customThe reaction
  5. customupon which the reaction
  6. filtrationfiltered through a phase separator
  7. concentrationconcentrated
  8. customcompletion of the reaction
  9. customthe product may be obtained
  10. customorganic chemistry techniques of workup and purification