反应 #3418728
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04954339
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Geranylbromide (20 g) in ethanol (50 ml) was added to 33% dimethylamine in industrial methylated spirits (240 ml) and the mixture was heated at reflux for 8 hours. The reaction mixture was evaporated to dryness, mixed with 2N sodium hydroxide (50 ml) and then extracted with diethyl ether (2×100ml). The ether extracts were combined and washed with water (50 ml), then dried with anhydrous magnesium sulphate and evaporated to dryness. The resulting orange oil was purified by chromatography (with a gradient CH2Cl2 :MeOH system as eluent) to give 1-dimethylamino-3.7-dimethyl-2,6-octadiene as an oil (12.1 g, 72%). the mixture was heated at reflux for 8 hours The reaction mixture was evaporated to dryness mixed with 2N sodium hydroxide (50 ml) extracted with diethyl ether (2×100ml) washed with water (50 ml) dried with anhydrous magnesium sulphate evaporated to dryness The resulting orange oil was purified by chromatography (with a gradient CH2Cl2
来源 ID: ord-ca449181923b4f8b8c11ce451cce48b7