HRID4180

反应详情

EQUATION

反应方程式

HRID 4180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

According to the method of Example 5, 1-methyl-2-chloromethyl-5-(2'-fluorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine (200 mg, 0.66 mmole) and m-trifluoromethyl aniline (319 mg, 1.97 mmole) were combined in 2 ml of dry N,N-dimethylformamide, and potassium carbonate (273 mg, 1.97 mmole) and sodium iodide (198 mg, 1.32 mmole) were added to this mixture (which was heated at 65° C. for 18 hours). After solvent-removal, partitioning, separation, washing, drying and concentrating, the analytical product was obtained via chromatography on silica gel (ethyl acetate-hexane elution, 3:7 v/v) and was shown to be 96% pure by HPLC.

WORKUP

后处理

  1. customAfter solvent-removal
  2. custompartitioning
  3. customseparation
  4. washwashing
  5. customdrying
  6. concentrationconcentrating
  7. customthe analytical product was obtained via chromatography on silica gel (ethyl acetate-hexane elution, 3:7 v/v)