反应详情

温度

110 °C

Combine 2-methyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride (600.0 mg, 2.31 mmol), (S)-2-(2-methoxy-ethyl)-piperazine (666.3 mg, 4.62 mmol), N,N-diisopropylethylamine (298.6 mg, 2.31 mmol), DMSO (1.0 ml), and toluene (4.0 ml) and stir and heat the mixture at 110° C. After 46 hours, cool the mixture to ambient temperature and dilute with ethyl acetate. Wash the organic layer with 0.1N 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 425.5 mg (53%) of a yellow foam: mp 63° C., dec; mass spectrum (ion spray): m/z 351.2 (M+1).

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