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Lithium Hydroxide → 2-(6-(1-((S)-3-(tert-butoxycarbonylamino)pyrrolidin-1-yl)-2,2,2-trifluoroethyl)-[1,2,4]triazolo[4,3-a]pyridin-3-yl)quinoline-7-carboxylic acid

HRID 338862
ノート
印刷プレビュー

反応式

HRID 338862 の反応式
[F:1][C:2]([F:26])([F:25])[CH:3]([N:12]1[CH2:16][CH2:15][C@H:14]([NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:13]1)[C:4]1[CH:5]=[N:6][C:7]([NH:10][NH2:11])=[CH:8][CH:9]=1.[CH:27]([C:29]1[CH:38]=[CH:37][C:36]2[C:31](=[CH:32][C:33]([C:39]([O:41]C)=[O:40])=[CH:34][CH:35]=2)[N:30]=1)=O.C(O)(=O)C.C(O)(=O)C.IC1C=CC=CC=1.C(=O)(O)[O-].[Na+].[Li+].[OH-]>CCO.C1COCC1.CCOCC.C(OCC)(=O)C>[C:20]([O:19][C:18]([NH:17][C@H:14]1[CH2:15][CH2:16][N:12]([CH:3]([C:4]2[CH:9]=[CH:8][C:7]3[N:6]([C:27]([C:29]4[CH:38]=[CH:37][C:36]5[C:31](=[CH:32][C:33]([C:39]([OH:41])=[O:40])=[CH:34][CH:35]=5)[N:30]=4)=[N:11][N:10]=3)[CH:5]=2)[C:2]([F:25])([F:1])[F:26])[CH2:13]1)=[O:24])([CH3:22])([CH3:23])[CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 3939Lithium HydroxideHCID 516892Sodium BicarbonateHCID 12217721Iodo benzene diacetateHCID 86707403tert-butyl (3S)-1-(2,2,2-trifluoro-1-(6-hydrazinylpyridin-3-yl)ethyl)pyrrolidin-3-ylcarbamateHCID 86707420Methyl 2-formylquinoline-7-carboxylate

生成物 1

HCID 70984597
2-(6-(1-((S)-3-(tert-butoxycarbonylamino)pyrrolidin-1-yl)-2,2,2-trifluoroethyl)-[1,2,4]triazolo[4,3-a]pyridin-3-yl)quinoline-7-carboxylic acid
収率 78.5%

試薬・触媒・溶媒 4

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of tert-butyl (3S)-1-(2,2,2-trifluoro-1-(6-hydrazinylpyridin-3-yl)ethyl)pyrrolidin-3-ylcarbamate (Example 1, Step D; 0.46 g, 1.03 mmol) and methyl 2-formylquinoline-7-carboxylate (0.22 g, 1.03 mmol) in EtOH (10 mL) was stirred at ambient temperature for 1 hour. The solvent was removed under reduced pressure. The residue was dissolved in DCM (10 mL) and iodo benzene diacetate (0.40 g, 1.24 mmol) was added. The mixture was stirred at ambient temperature for 1 hour. Ethyl acetate (20 mL) and saturated sodium bicarbonate (10 mL) were added. The organic layer was separated, washed with brine, dried (sodium sulfate), filtered and concentrated under reduced pressure. The residue obtained was dissolved in THF (5 mL) and 2 N LiOH (5.15 mL, 10.30 mmol) was added. The mixture was stirred at ambient temperature for 6 hours. Ether (20 mL) was added. The aqueous layer was separated and acidified with saturated potassium hydrogen sulfate to about pH 3. The resulting solid was collected by filtration to give 2-(6-(1-((S)-3-(tert-butoxycarbonylamino)pyrrolidin-1-yl)-2,2,2-trifluoroethyl)-[1,2,4]triazolo[4,3-a]pyridin-3-yl)quinoline-7-carboxylic acid (0.45 g, 78.5%) as a solid.

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in DCM (10 mL)
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried (sodium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue obtained
  9. stirringThe mixture was stirred at ambient temperature for 6 hours
  10. customThe aqueous layer was separated
  11. filtrationThe resulting solid was collected by filtration

出典と根拠

ORDレコード
ord-8a60f1f95e5741f7b39ce5247af7de02
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08889704B2

反応ノート

読み込み中…

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