反应 #3662242
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06215004B1
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a mechanically stirred suspension of P2O5 (42.53 g, 150 mmol) in dry DCM (100 ml) at 0° C., was slowly added 30 (11.0 g, 83 mmol), followed by DMSO (13 g, 11.8 ml, 166 mmol). After stirring at 0° C. for 1 h, the ice bath was removed and the mixture further stirred at ii for 1.5 h. It was then cooled to 0° C., and then Et3N (42 g, 58 ml, 416 mmol) was slowly added. The reaction was then left with stirring for 6 hours at room temperature. The reaction was quenched by adding 1.0 M HCl (60 ml) at 0° C., and left with stirring for 30 minutes at 0° C. The organic layer was then washed with water (2×250 ml), dried, filtered and evaporated to afford 24 (6.60 g, 51 mmol, 61%) as a yellow liquid, that was used in the next step without any further purification. the ice bath was removed the mixture further stirred at ii for 1.5 h It was then cooled to 0° C. The reaction was then left with stirring for 6 hours at room temperature The reaction was quenched by adding 1.0 M HCl (60 ml) at 0° C. left with stirring for 30 minutes at 0° C The organic layer was then washed with water (2×250 ml) dried filtered evaporated
来源 ID: ord-fb484b7edfc3411a9d94d28e94367f5f