Ethanol → HCID 54125530, compound

Temperature

60 °C

(S)-N,N-Diethyl-2-chloropropionamide (88.3 g) dissolved in ethanol (150 cc) is added to a suspension of the potassium salt of thiolacetic acid (72.6 g) in ethanol (300cc). The reaction mixture is then heated for 2 hours at a temperature in the vicinity of 60° C. and then filtered and concentrated to dryness under reduced pressure (130 Pa) at a temperature in the vicinity of 50° C. The residue obtained is taken up and stirred in dichloromethane (500 cc) and then washed with distilled water (300 cc), with a 10% aqueous potassium bicarbonate solution (300 cc) and then with distilled water (300 cc). The organic phase is decanted, dried over sodium sulphate and charcoal 3S (1 g) 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). (R)-N,N-Diethyl-2-acetylthiopropionamide (105.5 g) in the form of a slightly yellow oil [b.p.17Pa =105°-107° C.; [α]D20 =+156° (c=18.1 ; CHCl3)] is thereby obtained.

1. filtrationfiltered
2. concentrationconcentrated to dryness under reduced pressure (130 Pa) at a temperature in the vicinity of 50° C
3. customThe residue obtained
4. washwashed with distilled water (300 cc), with a 10% aqueous potassium bicarbonate solution (300 cc)
5. customThe organic phase is decanted
6. dry with materialdried over sodium sulphate and charcoal 3S (1 g)
7. filtrationfiltered
8. concentrationconcentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the vicinity of 30° C
9. customThe residue obtained
10. distillationis distilled under reduced pressure (17 Pa)

ORD record

ord-c6b680e46acb4d3fb7559f33ba255b31

Source dataset

uspto-grants-1988_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04775753