Ethyl Acetate → Lorazepam

HRID 1700799

Reaktionsgleichung

Reaktionsgleichung von HRID 1700799
[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>C1(C)C=CC=CC=1>[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 94,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Lorazepam ethanol solvate (100 g) was suspended in a 1:1 mixture of ethyl acetate and toluene (400 ml). The suspension was heated to 60° C. for 1 hour with rapid stirring and then cooled to 15° C. The suspension was filtered to recover the lorazepam. The lorazepam crystals were then washed with ethyl acetate (20 ml) and dried under 65 mm Hg vacuum at about 50° C. for about two hours to give crystalline lorazepam (83 g) in 88% yield.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-639a7eb95e2a4bee901453557bc86718
Quelldatensatz
uspto-grants-2002_02
Patentnummer
US06350870B2

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