反应详情

0.5 g (2.7 mmol) of 1-vinyl-1-cyclodecanol (cf. I.1.3, comprises also about 8-10% cyclodecanone), quartz reactor 25/400 mm, temperature 670° C.±10, vaporization at 95-100° C. (airbath temperature) in about 10 min. Nitrogen stream about 2-2.5 l/h, vacuum 5-6 mbar. 0.45 g (90% crude yield) of a pure white condensate were obtained which partially crystallized into small fine needles. According to GC and GC/MS analyses, the mixture comprises, as main component, about 70% cyclododecanone, as well as 6-8% cyclodecanone and 2-3% starting material. Chromatographic separation of the mixture over silica gel (hexane/TBME 97:3) gave 0.26 g of cyclododecanone (52% isolated yield), which has identical retention times and spectroscopic properties as the commercially available compound (Fluka).

1. custom400 mm, temperature 670° C.
2. customat 95-100° C.
3. customin about 10 min
4. custom0.45 g (90% crude yield) of a pure white condensate were obtained which
5. custompartially crystallized into small fine needles
6. customChromatographic separation of the mixture over silica gel (hexane/TBME 97:3)