反应 #3668638
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04895865
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A three neck 300 ml flask fitted with a reflux condenser, thermometer and dropping funnel was charged with 18.52 grams (0.15 moles) of commercially available 2-ethoxy benzylcyanide in 50 ml of dimethyl sulfoxide (DMSO). To the reaction was added 17.6 grams (0.165 moles, 1.1 ec.) of 1-chloropentane. While stirring at room temperature, 13.2 grams (0.165 moles) of 50% NaOH in 20 ml of DMSO was added over 20 minutes. A slight exotherm occurred and the reaction mixture was stirred at room temperature for 2 hours after which gas-liquid chromatoqraphy (GLC) indicated the reaction was 92% complete. The reaction was stirred for an additional 3 hours, then water was added followed by 200 ml of ether. After washing with acid and brine, the solvent was concentrated and gave an oil which was distilled under vacuum (160°-165° C. at 0.5 mm) and gave 15.82 grams (47.7% yield) of product. A three neck 300 ml flask fitted with a reflux condenser the reaction mixture was stirred at room temperature for 2 hours after which gas-liquid chromatoqraphy (GLC) The reaction was stirred for an additional 3 hours After washing with acid and brine the solvent was concentrated gave an oil which was distilled under vacuum (160°-165° C. at 0.5 mm)
来源 ID: ord-d969d0c05ac54f4e988d2585848262ab