反応 #4276

反応方程式

1-methyl-2-chloromethyl-5-(2'-fluorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine

m-trifluoromethyl aniline

potassium carbonate

sodium iodide

→

1-methyl-2-(3'-trifluoromethylphenyl)aminomethyl-5-(2'-fluorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   その他After solvent-removal
2. 2
   その他partitioning
3. 3
   その他separation
4. 4
   洗浄washing
5. 5
   その他drying
6. 6
   濃縮concentrating
7. 7
   その他the analytical product was obtained via chromatography on silica gel (ethyl acetate-hexane elution, 3:7 v/v)

実験手順

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.

出典