Formic Acid → HCID 54360432, compound

Participants

Reaction Conditions

Reaction Steps

To 110.7 g of above described N-benzyl-isoleucine (0.50 mol) were added 69.0 g formic acid (1.50 mol) and 49.4 g formaldehyde 36.5% in water (0.60 mol) and the clear, colorless reaction mixture was heated under stirring to ˜90° C. for 2 h. The reaction mixture was concentrated by rotary evaporation (60° C./25 mbar) and the residue was triturated under stirring (˜15 min) with 250 ml acetone. After evaporation of the solvent, triturating was repeated twice using a total of 500 ml acetone. Evaporation of the solvent (50° C./10 mbar) gave 129.9 g white, crystalline residue which was stirred with 200 ml acetone for 1 h at RT and 3 h at −20° C. The crystal suspension was filtered, washed with cold acetone and dried (16 h/50° C./10 mbar) affording 103.9 g (88.3%) product as a white, crystalline powder.

Provenance & Evidence