Lopinavir → Lopinavir cyclohexane

HRID 2093560ノート

反応式

HRID 2093560 の反応式
[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

参加物

4

反応物 1

HCID 92727Lopinavir

生成物 1

HCID 46866070Lopinavir cyclohexane収率 167.6%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8078Cyclohexane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7761202f64bb47d29d21beac7d488366
出典データセット
uspto-grants-2013_05
特許番号
US08445506B2

反応ノート

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