反应详情

温度

-70 °C

100 mg (0.76 mmol) of oxalyl chloride in 5 ml of dichloromethane are treated dropwise at −70° C. with 130 mg (1.64 mmol) of dimethyl sulphoxide. The mixture is stirred at −70° C. for 30 min, then 280 mg (0.63 mmol) of N-{1-[3-(3,4-dimethoxybenzyl)-5-oxo-4,5-dihydro-1,2,4-triazin-6-yl]ethyl}-2-(1-hydroxyethyl)-6-heptenamide (Example 29A) are added. After a further 30 min, during which the temperature in the batch rises to about −60° C., 320 mg (3.15 mmol) of triethylamine are added and the cooling bath is then removed. If the batch temperature is warmed almost to room temperature, 10 ml of water are added and the phases are separated after stirring briefly. The dried organic phase is chromatographed in dichloromethane/methanol 50/1.

1. waitAfter a further 30 min
2. customrises to about −60° C.
3. customthe cooling bath is then removed
4. temperatureIf the batch temperature is warmed almost to room temperature
5. addition10 ml of water are added
6. customthe phases are separated
7. stirringafter stirring briefly
8. customThe dried organic phase is chromatographed in dichloromethane/methanol 50/1