Lopinavir → Lopinavir cyclohexane

HRID 2093560노트

반응식

HRID 2093560 반응식
[CH3:1][C:2]1[C:7]([O:8][CH2:9][C:10]([NH:12][C@H:13]([C@@H:21]([OH:45])[CH2:22][C@@H:23]([NH:31][C:32]([C@@H:34]([N:38]2[C:43](=[O:44])[NH:42][CH2:41][CH2:40][CH2:39]2)[CH:35]([CH3:37])[CH3:36])=[O:33])[CH2:24][C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH2:14][C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)=[O:11])=[C:6]([CH3:46])[CH:5]=[CH:4][CH:3]=1>ClCCl.C1CCCCC1>[CH3:46][C:6]1[C:7]([O:8][CH2:9][C:10]([NH:12][C@H:13]([C@@H:21]([OH:45])[CH2:22][C@@H:23]([NH:31][C:32]([C@@H:34]([N:38]2[C:43](=[O:44])[NH:42][CH2:41][CH2:40][CH2:39]2)[CH:35]([CH3:37])[CH3:36])=[O:33])[CH2:24][C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH2:14][C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)=[O:11])=[C:2]([CH3:1])[CH:3]=[CH:4][CH:5]=1.[CH2:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1

참가 물질

4

반응물 1

HCID 92727Lopinavir

생성물 1

HCID 46866070Lopinavir cyclohexane수율 167.6%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8078Cyclohexane용매2회

실험 절차

Lopinavir (10 gm) was dissolved in dichloromethane (90 ml), methylenedichloride layer was dried over sodium sulfate and distilled off the solvent under vacuum at 45 deg C. to obtain residue. To the residue was added cyclohexane (50 ml), distilled off the solvent and the residue was collected. The residue obtained was taken in cyclohexane (70 ml), stirred for 60 hours at 20-25 deg C., filtered, washed the solid with cyclohexane (20 ml) and dried at 55-60 deg C. for 4 hours to obtain 9.5 gm of lopinavir cyclohexane solvate.

후처리

  1. dry with materialmethylenedichloride layer was dried over sodium sulfate
  2. distillationdistilled off the solvent under vacuum at 45 deg C
  3. customto obtain residue
  4. distillationdistilled off the solvent
  5. customthe residue was collected
  6. customThe residue obtained
  7. filtration, filtered
  8. washwashed the solid with cyclohexane (20 ml)
  9. customdried at 55-60 deg C

출처 및 근거

ORD 기록
ord-7761202f64bb47d29d21beac7d488366
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445506B2

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