反应 #3738606
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05827891
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a cold (0° C.) solution of 139.2 g (0.9 mol) of o-toluoyl chloride in 1200 mL of methylene chloride at 25° C., under nitrogen, was slowly added 180.0 g (1.8 mol) of triethylamine followed by the dropwise addition of a solution containing 73.14 g (1.0 mol) of t-butylamine in 200 mL of methylene chloride. The resulting reaction mixture was warmed to room temperature and allowed to react for 2.5 hours. The reaction mixture was then diluted with 1800 mL of water. The resulting organic and aqueous layers were separated, and the organic layer was washed sequentially with 2N sodium hydroxide, 1.0N hydrochloric acid and brine, dried over magnesium sulfate, filtered and then reduced to dryness under reduced pressure to provide 167.6 g of the desired subtitled compound as an off-white solid (mp 77°-78° C.). at 25° C. followed by the dropwise addition of a solution The resulting reaction mixture to react for 2.5 hours The resulting organic and aqueous layers were separated the organic layer was washed sequentially with 2N sodium hydroxide, 1.0N hydrochloric acid and brine dried over magnesium sulfate filtered
来源 ID: ord-5196e6d6be534c39b9007841eecea447