反应 #1080595
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04277498
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a suspension of (±)-N-(2-cyclohexyl-1-methylethyl)-2-phthalimidoacetamide (12.0 g, 36.7mmol) in ethanol (180 ml) was added hydrazine hydrate (2.05 g, 40.3 mmol) and the mixture heated under reflux for 1.5 hours. After cooling and standing at 0° for 24 hours, the slurry was filtered and the residue washed with petrol (40°-60°). The combined filtrateswere evaporated to dryness and the oily residue triturated with petrol (3×100 ml). The combined extracts were evaporated to dryness to givea colourless oil. The oil was dissolved in ether (50 ml) and the solution added to a warm solution of fumaric acid (2.7 g) in ethanol (50 ml). On standing, a colourless solid was deposited, m.p. 132°-134° C. the mixture heated under reflux for 1.5 hours After cooling the slurry was filtered the residue washed with petrol (40°-60°) The combined filtrateswere evaporated to dryness the oily residue triturated with petrol (3×100 ml) The combined extracts were evaporated to dryness The oil was dissolved in ether (50 ml) the solution added to a warm solution of fumaric acid (2.7 g) in ethanol (50 ml)
来源 ID: ord-8d4e06da135243daafe82bb006255f54