反应详情

温度

130 °C

To a solution of 106 mg (0.2 mmol) (RS)-1-(3,5-bis-trifluoromethyl-benzyl)-3-(3,4-dichloro-benzyl)-5-thioxo-[1,4]diazepan-2-one in 1 ml of butan-1-ol 42 mg (0.24 mmol) of 3-morpholin-4-yl-propionic acid hydrazide was added. The reaction mixture was stirred at 130° C. overnight. After evaporation of the solvent in vacuum water (5 ml) was added and the mixture was extracted three times with ethyl acetate. The combined organic layers are dried (MgSO4) and concentrated. The residue was purified by column chromatography (SiO2, dichloromethane/methanol=95:5) to yield 77 mg (59.2%) of the title compound as a light yellow solid. MS m/e (%): 650.0 (M+H+, 100).

1. customAfter evaporation of the solvent in vacuum water (5 ml)
2. additionwas added
3. extractionthe mixture was extracted three times with ethyl acetate
4. dry with materialThe combined organic layers are dried (MgSO4)
5. concentrationconcentrated
6. customThe residue was purified by column chromatography (SiO2, dichloromethane/methanol=95:5)