反应 #3547649
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07863475B2
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 N-(2,6-Dimethylbenzyl)phthalimide (Step B, 7.77 g, 29.3 mmol) in ethanol (80 ml) was added hydrazine monohydrate (2.16 ml, 44.52 mmol) and the reaction mixture was refluxed for 3.5 hours. To this reaction mixture was added c HCl to bring pH to 1 and refluxing continued for another 3.5 hours, water was added and reaction mixture was filtered, the filtrate was concentrated and pH was adjusted to 10 with 2 N NaOH. The residue was taken in methylene chloride and washed with brine, dried over Na2SO4, filtered and concentrated to give an oil which was used without further purification. the reaction mixture was refluxed for 3.5 hours refluxing reaction mixture was filtered the filtrate was concentrated washed with brine dried over Na2SO4 filtered concentrated to give an oil which was used without further purification
来源 ID: ord-e062a5fa6f5848f59c0e928c3e90517c