Chloroacetyl chloride → 2-chloro-N-cyclohexyl-N-ethylacetamide

N-Ethyl-cyclohexylamine (2.6 g) is dissolved in dry benzene (20 ml). To the solution are added dropwise with stirring chloroacetyl chloride (2.6 g) and triethylamine (2.4 g) under ice-cooling. The mixture is stirred under ice-cooling for one hour and further at room temperature for one hour. The reaction mixture is poured onto ice-water and extracted with ether. The ether layer is washed with an aqueous sodium hydrogen carbonate solution and an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After distilling off the solvent, the resulting residue is distilled under reduced pressure to give N-ethyl-N-cyclohexyl-chloroacetamide (3 g), b.p. 118°-120° C./0.2 mmHg.

1. temperaturecooling
2. additionThe reaction mixture is poured onto ice-water
3. extractionextracted with ether
4. washThe ether layer is washed with an aqueous sodium hydrogen carbonate solution
5. dry with materialan aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate
6. distillationAfter distilling off the solvent
7. distillationthe resulting residue is distilled under reduced pressure

ORDレコード

ord-242925c016684157afcee4b84035d296

出典データセット

uspto-grants-1985_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04540703