tert-butyl N-[3-(chloromethyl)phenyl]carbamate

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

实验步骤: While a solution of hydrazine monohydrate (1.32 g, 26.4 m mol) in ethanol (20 ml) was heated under reflux, a solution of 3-tert-butoxycarbonylaminobenzyl chloride (1.06 g, 4.4 m mol) in ethanol (10 ml) was added dropwise thereto over a period of 5 minutes. After this mixture was further refluxed for 0.5 hour, the solvent was distilled off under reduced pressure. The resulting oily residue was extracted with ether (2×20 ml). After the extract was concentrated under reduced pressure, the resulting residue was subjected to chromatography on silica gel (50 g) using chloroform-methanol (10:1), so that the desired compound (0.91 g, 87%) was obtained as an oily material. under reflux After this mixture was further refluxed for 0.5 hour the solvent was distilled off under reduced pressure The resulting oily residue was extracted with ether (2×20 ml) After the extract was concentrated under reduced pressure