Ketorolac → Ketorolac Tromethamine

HRID 636077

반응식

HRID 636077 반응식
[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]

참가 물질

4

반응물 2

HCID 3826KetorolacHCID 6503Tris(hydroxymethyl)aminomethane

생성물 1

HCID 84003Ketorolac Tromethamine

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
10 °C

실험 절차

Ketorolac acid (20 gm, Abbott Laboratories) was dissolved in 145 mL isopropanol. In a separate container, 10 gm of tromethamine (Aldrich Chemical Co.) was dissolved in 20 mL distilled water. The two mixtures were combined, mixed for 30 minutes then vacuum distilled under heat. Distillation was continued until approximately one half the volume remained, e.g., about 80 mL. Isopropanol (145 mL) was added and distillation continued until one half the volume remained, whereupon 270 mL of ethyl acetate was added and distillation of the ternary mixture continued. Upon removal of one-half the distillate, the ethyl acetate addition was repeated. When the volume was again brought to one half the starting volume, distillation was terminated. The solution was cooled to 10° C. and the solid ketorolac tromethamine isolated by filtration. The collected solids were dried under vacuum to afford 25 gm of the desired product. HPLC analysis showed purity of >99% of the desired compound.

후처리

  1. distillationdistilled water
  2. additionmixed for 30 minutes
  3. distillationvacuum distilled
  4. temperatureunder heat
  5. distillationDistillation
  6. additionIsopropanol (145 mL) was added
  7. distillationdistillation
  8. additionwas added
  9. distillationdistillation of the ternary mixture
  10. customUpon removal of one-half the distillate
  11. additionthe ethyl acetate addition
  12. distillationthe starting volume, distillation
  13. customwas terminated

출처 및 근거

ORD 기록
ord-a11c6095382e40e7944e16a4b855bfd3
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191285B1

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