反应详情

温度

60 °C

3.00 g (5.30 mmol) of the compound from example 13A was dissolved in 120 ml dichloromethane. 1.92 g (5.30 mmol) S-Trityl-L-cysteinamide, 0.92 ml (5.30 mmol) N,N-diisopropylethylamine and 2.02 g (5.30 mmol) HATU were added. The reaction mixture was split into 6 portions. The portions were heated for 30 min in a sealed tube at 60° C. in a microwave synthesizer. From the combined reaction mixture the solvent was removed by rotary evaporation (approx. 40° C., approx. 200 mbar, approx. 30 min.). The raw product was dissolved in dichloromethane and chromatographed over approx. 800 ml silica gel. Solvents used were dichloromethane/ethyl acetate 2/1, dichloromethane/ethyl acetate 1/1. The product-containing fractions were combined and concentrated to dryness under reduced pressure. This gave 4.91 g (3.73 mmol, 70% of theory, 69% purity) of the desired product.

1. customThe reaction mixture was split into 6 portions
2. customFrom the combined reaction mixture the solvent
3. customwas removed by rotary evaporation (approx. 40° C., approx. 200 mbar, approx. 30 min.)
4. dissolutionThe raw product was dissolved in dichloromethane
5. customchromatographed over approx. 800 ml silica gel
6. concentrationconcentrated to dryness under reduced pressure