Reaction #3246229
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04775753
Conditions: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: Diethylamine (480 cc) is added to a solution of (S)-2-chloropropionyl chloride (175.2 g) in chloroform (900 cc), which is maintained at 0° C., in the course of 1 hour. Distilled water (400 cc) and dichloromethane (300 cc) are added to the reaction mixture. The organic phase is decanted and then washed with an aqueous 2N hydrochloric acid solution (300 cc) and then with distilled water (400 cc). The organic phase is dried over sodium sulphate, filtered and then concentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the vicinity of 30° C. The residue obtained is distilled under reduced pressure (17 Pa). (S)-N,N-Diethyl-2-chloropropionamide (161.9 g) in the form of a colourless oil [b.p.17Pa =83°-85° C.; [α]D20 =+39.7°(c=10.4 ; CHCl3)] is thereby obtained. The organic phase is decanted washed with an aqueous 2N hydrochloric acid solution (300 cc) The organic phase is dried over sodium sulphate filtered concentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the vicinity of 30° C The residue obtained is distilled under reduced pressure (17 Pa)
Source ID: ord-b6cd0e4dc0a740fbafd072e442208f53