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Acetonitrile → 5-Amino-7-{3-(R)-[1-amino-1-(2-pyridyl)methyl]-1-pyrrolidinyl}-6,8-difluoro-1-[(1R,2S)-2-fluorocyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

HRID 457414
ノート
印刷プレビュー

反応式

HRID 457414 の反応式
C(OC([NH:8][CH:9]([C@@H:16]1[CH2:20][CH2:19][NH:18][CH2:17]1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1)=O)(C)(C)C.C(#N)C.[NH2:24][C:25]1[C:34]([F:35])=[C:33](F)[C:32]([F:37])=[C:31]2[C:26]=1[C:27](=[O:45])[C:28]([C:42]([OH:44])=[O:43])=[CH:29][N:30]2[C@@H:38]1[CH2:40][C@@H:39]1[F:41]>C(N(CC)CC)C>[NH2:24][C:25]1[C:34]([F:35])=[C:33]([N:18]2[CH2:19][CH2:20][C@@H:16]([CH:9]([NH2:8])[C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=3)[CH2:17]2)[C:32]([F:37])=[C:31]2[C:26]=1[C:27](=[O:45])[C:28]([C:42]([OH:44])=[O:43])=[CH:29][N:30]2[C@@H:38]1[CH2:40][C@@H:39]1[F:41]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6342AcetonitrileHCID 155235655-amino-6,7,8-trifluoro-[(1R,2S)-2-fluorocyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acidHCID 207414003-(R)-[1-Tert-butoxycarbonylamino-1-(2-pyridyl)methyl]pyrrolidine

生成物 1

HCID 207414295-Amino-7-{3-(R)-[1-amino-1-(2-pyridyl)methyl]-1-pyrrolidinyl}-6,8-difluoro-1-[(1R,2S)-2-fluorocyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid収率 54%

試薬・触媒・溶媒

1
HCID 8471Triethylamine溶媒

実験手順

3-(R)-[1-Tert-butoxycarbonylamino-1-(2-pyridyl)methyl]pyrrolidine [F2] (0.535 mmol) was added to an acetonitrile suspension (5 ml) of 5-amino-6,7,8-trifluoro-1-[2-(S)-fluoro-1-(R)-cyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (169 mg, 0.534 mmol), and the mixture was heated under reflux for 19 hours in the presence of triethylamine (0.5 ml). After cooling, the solvent of the reaction solution was evaporated under a reduced pressure. The resulting residue was dissolved in chloroform (50 ml), this was washed with 10% citric acid (40 ml) and saturated brine (40 ml) and dried over anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure. The resulting residue was mixed with concentrated hydrochloric acid (5 ml) under ice-cooling, further mixed with 1 mol/l hydrochloric acid aqueous solution (5 ml) at roam temperature and then washed with chloroform (50 ml×5). This hydrochloric acid aqueous solution was adjusted to an alkaline liquid property by adding 10 mol/l sodium hydroxide aqueous solution and then stirred at room temperature for 1 hour. This suspension was adjusted to a liquid property of pH 7.4 by adding concentrated hydrochloric acid and 1 mol/l hydrochloric acid and then extracted with chloroform (150 ml×3). The resulting organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under a reduced pressure to obtain the crude title compound as light yellow crystals. This was purified by recrystallizing from ethanol to obtain 136 mg (54%) of the title compound.

後処理

  1. temperaturethe mixture was heated
  2. temperatureAfter cooling
  3. customthe solvent of the reaction solution was evaporated under a reduced pressure
  4. dissolutionThe resulting residue was dissolved in chloroform (50 ml)
  5. washthis was washed with 10% citric acid (40 ml) and saturated brine (40 ml)
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was evaporated under a reduced pressure
  8. additionThe resulting residue was mixed with concentrated hydrochloric acid (5 ml) under ice-
  9. temperaturecooling
  10. additionfurther mixed with 1 mol/l hydrochloric acid aqueous solution (5 ml) at roam temperature
  11. washwashed with chloroform (50 ml×5)
  12. additionby adding 10 mol/l sodium hydroxide aqueous solution
  13. additionby adding concentrated hydrochloric acid and 1 mol/l hydrochloric acid
  14. extractionextracted with chloroform (150 ml×3)
  15. dry with materialThe resulting organic layer was dried over anhydrous sodium sulfate
  16. customthe solvent was evaporated under a reduced pressure
  17. customto obtain the crude title compound as light yellow crystals
  18. customThis was purified
  19. customby recrystallizing from ethanol

出典と根拠

ORDレコード
ord-20d7d09c94cb43ab8a250715c17bf336
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07186843B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート