2-chloro-N-phenacylacetamide

反応条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Phenacyl chloroacetamide (22.6 g; 0.107 mole) was mixed with polyphosphoric acid (200 g) and the mass heated with stirring for 30 minutes at 150° C. The hot liquid was then poured with vigorous stirring into water (800 ml). The mixture so formed was extracted with 3 × 100 ml chloroform, the extracts washed by shaking with water and dried over magnesium sulphate. The CHCl3 was evaporated off and the remaining oil extracted with 400 ml boiling 60°-80°0 C. petroleum ether. The resultant solution was treated with decolourising charcoal to remove tarry matter and evaporated, giving a pale yellow oil which crystallized rapidly. Yield 18.8 g (91%) m.p. 70°-1° C. the mass heated The hot liquid was then poured The mixture so formed was extracted with 3 × 100 ml chloroform the extracts washed by shaking with water dried over magnesium sulphate The CHCl3 was evaporated off the remaining oil extracted with 400 ml boiling 60° The resultant solution was treated with decolourising charcoal to remove tarry matter evaporated giving a pale yellow oil which crystallized rapidly

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Chloroacetyl chloride (25 g; 0.226 mole) was added slowly to a stirred solution of phenacylamine hydrochloride (25.9 g; 0.151 mole) in anhydrous dimethylformamide (DMF) (80 ml) at room temperature. The internal temperature rose to ca. 40° C. The mixture was stirred for 4 hours after the addition and the bulk of the DMF evaporated under vacuum. The residue was treated with water (200 ml) and the crystalline precipitate collected, washed with water and dried. Yield 24.75 g (77%). m.p. 118°-119° C. rose to ca. 40° C after the addition the bulk of the DMF evaporated under vacuum The residue was treated with water (200 ml) the crystalline precipitate collected washed with water dried