The preparation of alanine and glycine oligopeptidyl-tRNA is described. The method involves a reaction between N-hydroxysuccinimide ester of mono-p-methoxytrityl-Glyn (n = 1-3) or mono-p-methoxytrityl-Alan (n = 1-5) and aminoacyl-tRNA and subsequent removal of the N-protecting group by mild acidic treatment (5% dichloroacetic acid at 4°). The acylation reaction was repeated up to 4 times resulting in the formation of oligopeptidyl-tRNA of the type Glyn aminoacyl-tRNA (n = 1-12) and Alan aminoacyl-tRNA (n = 1-9). © 1969.