1-氰基-N-甲基甲磺酰胺

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of 1-cyano-N-methylmethanesulfonamide (from step (b), 250 mg, 1.9 mmol) in tetrahydrofaran (5 ml) at 0-5° C. under an atmosphere of nitrogen was added sodium hydride (60% dispersion in mineral oil, 75 mg, 1.9 mmol) in one portion. The resulting slurry was stirred at 0-5° C. for 45 min, before benzyloxymethyl chloride (80% purity, 0.368 g, 1.9 mmol) in tetrahydrofuran (5 ml) was added dropwise over a 15 min period. The mixture was then allowed to warm to ambient temperature over a 3 hr period. The solvents were then evaporated in vacuo and the resulting oil was purified by flash column chromatography (diethyl ether:hexanes 3:1 as eluant) to yield the subtitle compound (296 mg, 61.6%) as a colourless oil. was added dropwise over a 15 min period The solvents were then evaporated in vacuo the resulting oil was purified by flash column chromatography (diethyl ether:hexanes 3:1 as eluant)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of 1-cyano-N-methylmethanesulfonamide (from step (b), 250 mg, 1.9 mmol) in tetrahydrofaran (5 ml) at 0-5° C. under an atmosphere of nitrogen was added sodium hydride (60% dispersion in mineral oil, 75 mg, 1.9 mmol) in one portion. The resulting slurry was stirred at 0-5° C. for 45 min, before benzyloxymethyl chloride (80% purity, 0.368 g, 1.9 mmol) in tetrahydrofuran (5 ml) was added dropwise over a 15 min period. The mixture was then allowed to warm to ambient temperature over a 3 hr period. The solvents were then evaporated in vacuo and the resulting oil was purified by flash column chromatography (diethyl ether:hexanes 3:1 as eluant) to yield the subtitle compound (296 mg, 61.6%) as a colourless oil. was added dropwise over a 15 min period The solvents were then evaporated in vacuo the resulting oil was purified by flash column chromatography (diethyl ether:hexanes 3:1 as eluant)