反应详情

温度

80 °C

0.931 g (1.92 mmol) of the compound from example 1A was dissolved in 30 ml dichloromethane. 0.455 g (1.92 mmol) of the compound from example 6A was added. The reaction mixture was split into 2 portions. The portions were heated for 30 min in a sealed tube at 80° C. in a microwave synthesizer. From the combined reaction mixture the solvent was removed under reduced pressure. The raw product was purified by preparative RP-HPLC on a C18 column with a water methanol gradient from 9/1 to 1/9. The product-containing fractions were combined and concentrated to dryness under reduced pressure. This gave 0.523 g (0.85 mmol, 44% of theory) of the desired product as a mixture of 2 diastereomers.

1. customThe reaction mixture was split into 2 portions
2. customFrom the combined reaction mixture the solvent
3. customwas removed under reduced pressure
4. customThe raw product was purified by preparative RP-HPLC on a C18 column with a water methanol gradient from 9/1 to 1/9
5. concentrationconcentrated to dryness under reduced pressure
6. additionThis gave 0.523 g (0.85 mmol, 44% of theory) of the desired product as a mixture of 2 diastereomers