反应详情

185 mg (0.37 mmol) of the compound from Example 42A and 50 mg (0.48 mmol) of ethyl N′-hydroxyimidocarbamate [G. Zinner, G. Nebel, Arch. Pharm. 1970, 303, 385-390] were initially charged in 1.0 ml of DMF and reacted with 210 mg (0.55 mmol) of HATU and 0.19 ml (143 mg, 1.1 mmol) of N,N-diisopropylethylamine. The mixture was stirred at RT for 15 minutes and then the reaction mixture was partitioned between water and ethyl acetate. The organic phase was washed repeatedly with water, dried over sodium sulphate and concentrated under reduced pressure. The residue was dissolved in 2.0 ml of acetic acid and heated to reflux for 1 h. The reaction mixture was purified by means of preparative HPLC. Yield: 62 mg (33% of theory)

1. customthe reaction mixture was partitioned between water and ethyl acetate
2. washThe organic phase was washed repeatedly with water
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated under reduced pressure
5. dissolutionThe residue was dissolved in 2.0 ml of acetic acid
6. temperatureheated
7. temperatureto reflux for 1 h
8. customThe reaction mixture was purified by means of preparative HPLC