反应详情

Combine (S)-10-[3-(2-methoxyethyl)piperazin-1-yl]-2-isopropyl 4H-3-thia-1,4,9-triazabenzo[f]azulene (0.103 g, 0.267 mmol), acetaldehyde (30 μL, 0.534 mmol), and sodium triacetoxyborohydride (0.085 g, 0.401 mmol) in dichloroethane (7 mL) and stir, at room temperature for 6 hours. Dilute the mixture with saturated aqueous sodium bicarbonate and extract three times with dichloromethane. Combine the organic layers, dry over sodium sulfate and concentrate under reduced pressure to give the crude product. Purification by flash chromatography, eluting with a step gradient starting with dichloromethane going to 5% 2N ammonia-methanol in dichloromethane, gives the free base of the title compound (0.79 g, 71%) as a yellow foam: mass spectrum (APCI): m/z=414.2 (M+1). Isolate clean product as the corresponding dihydrochloride in the manner described in Example 319. Exact Mass, Calc: 414.2328; Found: 414.2326.

1. extractionextract three times with dichloromethane
2. dry with materialdry over sodium sulfate
3. concentrationconcentrate under reduced pressure
4. customto give the crude product
5. customPurification by flash chromatography
6. washeluting with a step gradient