反应详情

A solution of 495 g (1710.6 mmol) of (4-Methoxymethylene-cyclohexyl)-methyl-carbamic acid benzyl ester in 1.7 l THF was treated with 3.42 l of aqueous 1N HCl at RT and heated at reflux for 2 h. The reaction was cooled to RT and extracted with TBME (1.7 and 0.9 l). The organic phase was washed with aqueous 1M NaHCO3, dried (Na2SO4), filtered and evaporated to give 457.4 (97%) of crude (4-Formyl-cyclohexyl)-methyl-carbamic acid benzyl ester (trans:cis ca 70:30).

1. temperatureheated
2. temperatureat reflux for 2 h
3. extractionextracted with TBME (1.7 and 0.9 l)
4. washThe organic phase was washed with aqueous 1M NaHCO3
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customevaporated