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With diethylamino-sulfur trifluoride In dichloromethane at 10℃; for 15.25h;
2 Synthesis of compound VIII:
1L single neck flask was added Intermediate (66.6g, 0.336mol, 1.0eq.), Dissolved with DCM (600mL), was added dropwise diethylamino sulfur trifluoride (81.2g, 0.504mol, 1.5eq.), at 10 °C , holding about 15min after dropping 10 °C reaction 15h, TLC the reaction was complete. The reaction solution was poured into 1L of stirring ice-water mixture, settled and separated, and the aqueous layer was washed with DCM (100mL × 1) and the combined DCM layers, then 1L of water, 1L saturated sodium bicarbonate, saturated sodium chloride, respectively 1L washed, the DCM layer was dried over anhydrous sodium sulfate, suction filtered, and concentrated to give 66.3 g light brown oil, sand column chromatography (PE ~ PE: EA = 10: 1) to give 59.3g pale yellow liquid, which solidified on standing theoretical yield: 67.27g, yield: 88.1%
Multi-step reaction with 3 steps
1: acetonitrile / 3 h / 60 °C
2: hydrogenchloride / ethyl acetate; water / 1 h / 0 °C
3: diethylamino-sulfur trifluoride / dichloromethane / 15.25 h / 10 °C
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