反应详情

温度

0 °C

Add a solution of fluoroacetyl chloride (0.133 g, 1.38 mmol) in anhydrous dichloromethane (1-2 mL) dropwise to a 0° C. solution of (S)-10-[3-(2-Methoxy-ethyl)-piperazin-1-yl]-2-trifluoromethyl-4H-3-thia-1,4,9-triaza-benzo[f]azulene (0.283 g, 0.688 mmol) and diisopropylethylamine (0.240 mL, 1.38 mmol) in anhydrous dichloromethane, and stir at 0° C. for 3 hours. Concentrate the reaction under reduced pressure to afford an oil. Purify the oil by flash chromatography, eluting with a gradient of a solution of 2% 2M ammonia in methanol, in dichloromethane (0-100% in dichloromethane over 30 minutes, then 100% for 28 minutes) to give the title compound: 0.18 g (56%). Mass spectrum (APCI+, m/e): 472 (M+1).

1. concentrationConcentrate
2. customthe reaction under reduced pressure
3. customto afford an oil
4. customPurify the oil by flash chromatography
5. washeluting with a gradient of a solution of 2% 2M ammonia in methanol, in dichloromethane (0-100% in dichloromethane over 30 minutes