反应详情

N6-[1-(hydroxyimino)ethyl]-2-methyl-lysine, dihydrochloride ##STR8## EX-3A) A suspension of lysine ethyl ester dihydrochloride (33 g; 0.14 mole) and MgSO4 (34 g; 0.28 moles) in a solution of 4-chloro-benzaldehyde (39 g; 0.28 moles) and acetonitrile (500 mL) was stirred while N,N-diisopropylethylamine (36 g; 0.28 moles) was added in portions over 1/2 h. The mixture was stirred for 12 h, filtered, concentrated to a small volume, and diluted with 500 mL of diethyl ether. The ether solution was washed with 0.1% aqueous NaHCO3, aqueous 2 N NaOH containing 2 g/100 ml of NH2OH.HCl, again with 0.1% aqueous NaHCO3 and saturated aqueous NaCl. After drying with MgSO4 and removal of the solvent in vacuo, ethyl N, N'-di(4-chloro-phenylmethylene)-L-lysine was obtained as a clear liquid.

1. additionwas added in portions over 1/2 h
2. filtrationfiltered
3. concentrationconcentrated to a small volume
4. additiondiluted with 500 mL of diethyl ether
5. washThe ether solution was washed with 0.1% aqueous NaHCO3, aqueous 2 N NaOH containing 2 g/100 ml of NH2OH.HCl, again with 0.1% aqueous NaHCO3 and saturated aqueous NaCl
6. dry with materialAfter drying with MgSO4 and removal of the solvent in vacuo