Ethanol → HCID 54125531, Verbindung

HRID 867612Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 867612
[CH2:1]([N:3]([CH2:9][CH3:10])[C:4](=O)[C@H:5](Cl)[CH3:6])[CH3:2].[K].[S:12]1C=CC=C1CC(O)=O.[CH2:21]([OH:23])[CH3:22]>ClCCl>[CH2:1]([N:3]([CH2:9][CH3:10])[C:4](=[S:12])[C@H:5]([C:21](=[O:23])[CH3:22])[CH3:6])[CH3:2]

Komponenten

6

Edukt 4

HCID 702Ethanol2×HCID 159702-Thiopheneacetic acidHCID 5462222PotassiumHCID 13318792HCID 13318792, Verbindung

Produkt 1

HCID 54125531HCID 54125531, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
55 °C

Versuchsvorschrift

(R)-N,N-Diethyl-2-chloropropionamide (20 g) dissolved in ethanol (30 cc) is added to a suspension of the potassium salt of thiolacetic acid (16 g) in ethanol (70 cc). The reaction mixture is then heated for 2 hours at a temperature in the vicinity of 55° C. and then concentrated to dryness under reduced pressure (130 Pa) at a temperature in the vicinity of 60° C. The residue obtained is crushed in dichloromethane (300 cc) and then washed with distilled water (200 cc). The organic phase is decanted, 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-acetylthiopropionamide (22 g) in the form of a slightly yellow oil [b.p.17Pa =105°-107° C.; [α]D20 =-169° (c=10; CHCl3)] is thereby obtained.

Aufarbeitung

  1. concentrationconcentrated to dryness under reduced pressure (130 Pa) at a temperature in the vicinity of 60° C
  2. customThe residue obtained
  3. washwashed with distilled water (200 cc)
  4. customThe organic phase is decanted
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the vicinity of 30° C
  8. customThe residue obtained
  9. distillationis distilled under reduced pressure (17 Pa)

Quellen und Nachweise

ORD-Eintrag
ord-d6f4a217e393461d9704f20f82ab1373
Quelldatensatz
uspto-grants-1988_10
Patentnummer
US04775753

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