반응 #1678440

반응 방정식

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

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타After solvent-removal
2. 2
   기타partitioning
3. 3
   기타separation
4. 4
   세척washing
5. 5
   기타drying
6. 6
   농축concentrating
7. 7
   기타the analytical product was obtained via chromatography on silica gel (ethyl acetate-hexane elution, 3:7 v/v)

실험 절차

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.

출처