反应详情

温度

60 °C

A solution of 4-((1,3-dioxoisoindolin-2-yl)methyl)-N,N,N′-trimethyl-benzene-sulfonimidamide (preparation 60c, 280 mg, 0.78 mmol) in a 2:1:1 mixture of acetonitrile, tetrahydrofuran and ethanol (8 mL) is treated with 1,2-diaminoethane (116 μL, 1.74 mmol). The mixture is heated at 60° C. for 5 h, and another portion of 1,2-diaminoethane (26 μL, 0.39 mmol) is added. After 1.5 h all volatiles are removed under reduced pressure. The residue is treated with dichloromethane, and the mixture is filtered. The filtrate is concentrated under reduced pressure. Yield: 172 mg (97% of theory). ESI mass spectrum: [M+H]+=228; r.t. HPLC: 0.66 min (V011_S01).

1. customAfter 1.5 h all volatiles are removed under reduced pressure
2. additionThe residue is treated with dichloromethane
3. filtrationthe mixture is filtered
4. concentrationThe filtrate is concentrated under reduced pressure
5. customr.t
6. custom0.66 min (V011_S01)