Ketorolac → Ketorolac Tromethamine

HRID 636078

Reaktionsgleichung

Reaktionsgleichung von HRID 636078
[CH:1]1[CH:2]=[CH:3][C:4]([C:7]([C:9]2[N:13]3[CH2:14][CH2:15][CH:16]([C:17]([OH:19])=[O:18])[C:12]3=[CH:11][CH:10]=2)=[O:8])=[CH:5][CH:6]=1.[NH2:20][C:21]([CH2:26][OH:27])([CH2:24][OH:25])[CH2:22][OH:23]>C(O)(C)C>[CH:1]1[CH:6]=[CH:5][C:4]([C:7]([C:9]2[N:13]3[CH2:14][CH2:15][CH:16]([C:17]([OH:19])=[O:18])[C:12]3=[CH:11][CH:10]=2)=[O:8])=[CH:3][CH:2]=1.[CH2:22]([OH:23])[C:21]([NH2:20])([CH2:26][OH:27])[CH2:24][OH:25]

Komponenten

4

Edukt 2

HCID 3826KetorolacHCID 6503Tris(hydroxymethyl)aminomethane

Produkt 1

HCID 84003Ketorolac Tromethamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

Ketorolac acid (10.0 gm, Abbott Laboratories) is dissolved in 75 mL isopropanol. In a separate container, 5.0 gm of tromethamine (Aldrich Chemical Co.) is dissolved in 10 mL distilled water. The two mixtures are combined, mixed for 30 minutes then distilled under atmosphereric conditions. Distillation is continued until approximately one half the volume remains, e.g., about 40 mL. Isopropanol (72 mL) is added and distillation continued until one half the volume remains, whereupon 135 mL of ethyl acetate is added and distillation of the ternary mixture continued. Upon removal of one-half the distillate, the ethyl acetate addition is repeated. When the volume is again brought to one half the starting volume, distillation is terminated. The solution is cooled to 10° C. and the solid ketorolac tromethamine isolated by filtration. The collected solids are dried under vacuum to afford the desired product.

Aufarbeitung

  1. distillationdistilled water
  2. additionmixed for 30 minutes
  3. distillationthen distilled under atmosphereric conditions
  4. distillationDistillation
  5. additionIsopropanol (72 mL) is added
  6. distillationdistillation
  7. additionis added
  8. distillationdistillation of the ternary mixture
  9. customUpon removal of one-half the distillate
  10. additionthe ethyl acetate addition
  11. distillationthe starting volume, distillation
  12. customis terminated

Quellen und Nachweise

ORD-Eintrag
ord-80f1727fc0b4422b98f3a8f8a66d2208
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06191285B1

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