PURPOSE: To prepare t-butyl carbamate in a high yield, by catalytically reducing a benzyl carbamate derivative in the presence of di-t-butyl dicarbonate on a palladium catalyst.

CONSTITUTION: The objective component of formula II is prepared by catalytical ly reducing a benzyl carbamate derivative of formula I [R represents an amino acid residue or peptide residue together with the imino group combined with the R (other groups of the amino acid residue and the peptide residue are protected with protecting groups used for the synthesis of peptides)] in the presence of di-t-butyl dicarbonate on a palladium catalyst (e.g., Pd-C) in a sol vent such as methanol or by reacting the compound of formula I with triethylsilane in the coexistence of the di-p-butyl dicarbonate and triethylamine on the palladium catalyst in an alcoholic solvent. Restrictions for the chemical stability against acids or bases on the synthesis of peptides, etc., are solvent and nitrogen-containing physiologically active substances can be therefore readily synthetized.