反应 #3342117
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06951964B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 5 g (23.8 mmol) of 1-vinylcyclododecanol, quartz reactor 25/400 mm, temperature 660° C.±10, vaporization at 125-135° C. (airbath temperature) in about 30 min. Nitrogen stream about 1-2 l/h, vacuum 4-6 mbar. The oily condensate began to crystallize in the cool trap already. 4.4 g (88% crude yield) of a wax-like solid were obtained which, according to GC and GC/MS analyses, comprises as well as 80-85% of the main component also up to about 5% cyclododecanone and about 5-10% other components which, according to the molecular masses found, are dehydrogenation products. Recrystallization twice from hexane at 0° and −20° C., gave 3.6 g (72%) of cyclotetradecanone (GC purity>98%) as colorless needles with a melting point of 56° C. to crystallize in the cool trap already 4.4 g (88% crude yield) of a wax-like solid were obtained which Recrystallization twice from hexane at 0°
来源 ID: ord-2619c7353c0f44839900ed27e14c07ff