Ethyl Acetate → Lorazepam

HRID 1700798

Reaktionsgleichung

Reaktionsgleichung von HRID 1700798
[CH:1]1[CH:2]=[CH:3][C:4]([Cl:21])=[C:5]([C:7]2[C:14]3[CH:15]=[C:16]([Cl:19])[CH:17]=[CH:18][C:13]=3[NH:12][C:10](=[O:11])[CH:9]([OH:20])[N:8]=2)[CH:6]=1.C(O)C.C(OCC)(=O)C>C1CCCCC1>[CH:1]1[CH:2]=[CH:3][C:4]([Cl:21])=[C:5]([C:7]2[C:14]3[CH:15]=[C:16]([Cl:19])[CH:17]=[CH:18][C:13]=3[NH:12][C:10](=[O:11])[CH:9]([OH:20])[N:8]=2)[CH:6]=1

Komponenten

4

Edukt 2

HCID 8857Ethyl AcetateHCID 18318790HCID 18318790, Verbindung

Produkt 1

HCID 3958LorazepamAusbeute 97,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8078CyclohexaneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Lorazepam ethanol solvate (100 g) was suspended in a 1:1 mixture of ethyl acetate and cyclohexane (800 ml). The suspension was heated to 60° C. for 1 hour with rapid stirring and then cooled to 15° C. The cooled suspension was filtered to recover the lorazepam crystals and the crystals were then washed with ethyl acetate (20 ml). The crystals were dried at 50° C. under 65 mm Hg vacuum for two hours to give crystalline lorazepam (85 g, 90%).

Aufarbeitung

  1. temperaturecooled to 15° C
  2. filtrationThe cooled suspension was filtered
  3. customto recover the lorazepam crystals
  4. washthe crystals were then washed with ethyl acetate (20 ml)
  5. customThe crystals were dried at 50° C. under 65 mm Hg vacuum for two hours

Quellen und Nachweise

ORD-Eintrag
ord-e77446ecc1754bb68f2c2868bde4cd7e
Quelldatensatz
uspto-grants-2002_02
Patentnummer
US06350870B2

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