Phosphoric Acid → HCID 88265334, compound

Participants

Reaction Steps

A solution of D-serinamide (0.01 moles, 1 g) and 4-heptanone (0.01 moles, 1.1 g) in methanol (50 ml) is added with 4M methanol HCl (0.0033 moles, 0.85 ml) and sodium cyanoborohydride (0.005 moles, 0.33 g). The mixture is reacted at r.t. for 10 days, acidified with methanol HCl to pH=2, and evaporated to dryness under vacuum. The residue is taken up with water (100 ml), washed with ethyl ether (100 ml), alkalinized with sodium carbonate and extracted with chloroform (3×100 ml). The resulting oil (1.3 g) is dissolved in methanol (50 ml) and treated with 85% phosphoric acid (0.0065 moles, 0.75 g), then evaporated to dryness under vacuum to obtain the product as a very light solid foam. Yield: 2 g (77%)--m.p.=150-156° C. ]589 (c=1, water)=+1.9

Provenance & Evidence