反应详情

温度

70 °C

100 mg (0.513 mmol) of 5-nitrobenzo[d]isothiazol-3-ylamine were suspended in 5 ml of THF. Addition of 78.1 mg (0.61 mmol) of 1-isocyanatohexane was followed by stirring at RT for 2 h and at 70° C. for 2 h. Then a further 0.3 mmol of 1-isocyanatohexane was added, and stirring was continued at 70° C. for 6 h. The reaction mixture was concentrated, and the residue was dissolved in water and extracted with ethyl acetate. The organic phase was concentrated and purified by preparative HPLC (PR18, acetonitrile/water 0.1% TFA). Yield: 18 mg (11%), M+H+: 323.15.

1. stirringstirring
2. waitwas continued at 70° C. for 6 h
3. concentrationThe reaction mixture was concentrated
4. dissolutionthe residue was dissolved in water
5. extractionextracted with ethyl acetate
6. concentrationThe organic phase was concentrated
7. custompurified by preparative HPLC (PR18, acetonitrile/water 0.1% TFA)