反应详情

温度

110 °C

Combine 3-methyl-5H-dibenzo[b,e][1,4]diazepin-1-ylamine hydrochloride (400.0 mg, 1.54 mmol), (S)-2-[2-(3-Fluoro-phenyl)-ethyl]-piperazine (641.5 mg, 3.08 mmol), N,N-diisopropylethylamine (199.0 mg, 1.54 mmol), DMSO (0.7 ml), and toluene (2.8 ml). Stir and heat the mixture at 110° C. After 64 hours, cool the mixture to ambient temperature and then dilute it with ethyl acetate. Wash the organic layer with 0.1 N NaOH and brine. Dry (sodium sulfate) and concentrate the organic layer to residue. Purify the residue on silica gel using dichloromethane/methanol (90:10) to give 423.2 mg (66%) of a tan foam: mp 81°, dec; mass spectrum (ion spray): m/z 415.2 (M+1).

1. temperaturecool the mixture to ambient temperature
2. washWash the organic layer with 0.1 N NaOH and brine
3. dry with materialDry (sodium sulfate)
4. concentrationconcentrate the organic layer to residue
5. customPurify the residue on silica gel