Water → Dexibuprofen lysine anhydrous

HRID 982187

반응식

HRID 982187 반응식
[OH:1][C:2]([CH:4]([C:6]1[CH:15]=[CH:14][C:9]([CH2:10][CH:11]([CH3:13])[CH3:12])=[CH:8][CH:7]=1)[CH3:5])=[O:3].[NH2:16][C@H:17]([C:23]([OH:25])=[O:24])[CH2:18][CH2:19][CH2:20][CH2:21][NH2:22].O>C(O)C>[OH:3][C:2]([C@H:4]([C:6]1[CH:7]=[CH:8][C:9]([CH2:10][CH:11]([CH3:12])[CH3:13])=[CH:14][CH:15]=1)[CH3:5])=[O:1].[NH2:16][C@H:17]([C:23]([OH:25])=[O:24])[CH2:18][CH2:19][CH2:20][CH2:21][NH2:22]

참가 물질

5

반응물 3

HCID 962WaterHCID 3672Ibuprofen, (+-)-HCID 5962L-Lysine

생성물 1

HCID 9819903Dexibuprofen lysine anhydrous수율 98.1%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
25 °C

실험 절차

167 grams of racemic ibuprofen and 118 grams of (S)-lysine were charged into 180 cc of water and 5.82 liters of ethanol were added. The resulting slurry was agitated and aged at 30° C. for 24 hours. A clear liquor was drawn off through a filter and the liquor cooled to 25° C. The resulting supersaturated liquor was then added to a slurry of 50 grams of 99.4% (S)-ibuprofen-(S)-lysine. The precipitated solid was separated by filtration and the mother liquor recycled to the slurry mixture of racemic ibuprofen and (S)-lysine. The procedure was continued until essentially all the (S)-ibuprofen in the original charge was depleted. This procedure resulted in the formation of 144 grams of 98.1-98.8% pure (S)-ibuprofen-(S)-lysine.

후처리

  1. additionwere added
  2. filtrationa filter
  3. additionThe resulting supersaturated liquor was then added to a slurry of 50 grams of 99.4% (S)-ibuprofen-(S)-lysine
  4. customThe precipitated solid was separated by filtration
  5. additionthe mother liquor recycled to the slurry mixture of racemic ibuprofen and (S)-lysine
  6. additionoriginal charge

출처 및 근거

ORD 기록
ord-8c4db727173c4390897c9f6ea3835f01
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04994604

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