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0 °C

A solution of 12.25 g (313.11 mmol) LAH in 1.3 l THF was cooled (−50° C.) and treated during 30 min with a solution of 89.5 g (284.64 mmol) of trans-[4-(Methoxy-methyl-carbamoyl)-cyclohexylmethyl]-methyl-carbamic acid tert-butyl ester in 1.3 l THF. After 20 min at this temperature, the reaction was warmed up to 0° C., cooled (−78° C.) and hydrolyzed with a suspension of 90 g MgSO4.7H2O, 90 g silicagel in 292 ml aqueous 10% KHSO4. The cooling bath was removed, THF was added, the mixture was stirred for 30 min and filtered. After evaporation, the residue was dissolved in CH2Cl2, dried over Na2SO4 and evaporated to yield 90.4 (quantitative) of trans-(4-Formyl-cyclohexylmethyl)-methyl-carbamic acid tert-butyl ester, MS: 255 (M).

1. temperaturecooled (−78° C.)
2. customThe cooling bath was removed
3. additionTHF was added
4. filtrationfiltered
5. customAfter evaporation
6. dissolutionthe residue was dissolved in CH2Cl2
7. dry with materialdried over Na2SO4
8. customevaporated