Water → HCID 13318791, compound

Temperature

0 °C

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.

1. customThe organic phase is decanted
2. washwashed with an aqueous 2N hydrochloric acid solution (300 cc)
3. dry with materialThe organic phase is dried over sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the vicinity of 30° C
6. customThe residue obtained
7. distillationis distilled under reduced pressure (17 Pa)

ORD record

ord-b6cd0e4dc0a740fbafd072e442208f53

Source dataset

uspto-grants-1988_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04775753