反应详情

温度

60 °C

1.50 g (2.59 mmol) of the compound from example 11A was dissolved in 60 ml dichloromethane. 0.940 g (2.59 mmol) S-Trityl-L-cysteinamide, 0.45 ml (2.60 mmol) N,N-diisopropylethylamine and 0.984 g (2.59 mmol) HATU were added. The reaction mixture was split into 3 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. 400 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 1.72 g (1.64 mmol, 63% of theory, 88% purity) of the desired product.

1. customThe reaction mixture was split into 3 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. 400 ml silica gel
6. concentrationconcentrated to dryness under reduced pressure