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(R)-tert-butyl 3-((5-tosyl-5H-pyrrolo[2,3-b]pyrazin-2-yl)methylcarbamothioyl)piperidine-1-carboxylate → (R)-tert-butyl 3-(6-tosyl-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)piperidine-1-carboxylate

HRID 1969782
ノート
印刷プレビュー

反応式

HRID 1969782 の反応式
[S:1]([N:11]1[C:15]2=[N:16][CH:17]=[C:18]([CH2:20][NH:21][C:22]([C@@H:24]3[CH2:29][CH2:28][CH2:27][N:26]([C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:25]3)=S)[N:19]=[C:14]2[CH:13]=[CH:12]1)([C:4]1[CH:10]=[CH:9][C:7]([CH3:8])=[CH:6][CH:5]=1)(=[O:3])=[O:2]>O1CCOCC1.FC(F)(F)C([O-])=O.[Hg+2].FC(F)(F)C([O-])=O>[S:1]([N:11]1[C:15]2[N:16]=[CH:17][C:18]3[N:19]([C:22]([C@@H:24]4[CH2:29][CH2:28][CH2:27][N:26]([C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:25]4)=[N:21][CH:20]=3)[C:14]=2[CH:13]=[CH:12]1)([C:4]1[CH:10]=[CH:9][C:7]([CH3:8])=[CH:6][CH:5]=1)(=[O:3])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 58557198(R)-tert-butyl 3-((5-tosyl-5H-pyrrolo[2,3-b]pyrazin-2-yl)methylcarbamothioyl)piperidine-1-carboxylate

生成物 1

HCID 58557605(R)-tert-butyl 3-(6-tosyl-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)piperidine-1-carboxylate収率 87%

試薬・触媒・溶媒 2

HCID 2723924Mercury bis(trifluoroacetate)触媒HCID 312751,4-Dioxane溶媒

実験手順

To a solution of (R)-tert-butyl 3-((5-tosyl-5H-pyrrolo[2,3-b]pyrazin-2-yl)methylcarbamothioyl)-piperidine-1-carboxylate (5.61 g, 10.3 mmol) in 1,4-dioxane (96 mL) was added mercury (II) trifluoroacetate (4.38 g, 10.3 mmol). The reaction mixture was stirred at ambient temperature for about 2 h then filtered through a pad of Celite®. The Celite® pad was rinsed with EtOAc (50 mL) and the filtrate was concd under reduced pressure. The crude residue was dissolved in EtOAc (40 mL) and the organic phase was washed with saturated aqueous NaHCO3 (2×40 mL) and brine (30 mL), dried over anhydrous MgSO4, filtered, and coned under reduced pressure. The crude material was purified by silica gel chromatography eluting with a gradient of 0-5% MeOH in DCM to afford (R)-tert-butyl 3-(6-tosyl-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)piperidine-1-carboxylate (4.4 g, 87%): LC/MS (Table 1, Method b) Rt=2.49 min; MS m/z: 496 (M+H)+.

後処理

  1. filtrationthen filtered through a pad of Celite®
  2. washThe Celite® pad was rinsed with EtOAc (50 mL)
  3. dissolutionThe crude residue was dissolved in EtOAc (40 mL)
  4. washthe organic phase was washed with saturated aqueous NaHCO3 (2×40 mL) and brine (30 mL)
  5. dry with materialdried over anhydrous MgSO4
  6. filtrationfiltered
  7. customThe crude material was purified by silica gel chromatography
  8. washeluting with a gradient of 0-5% MeOH in DCM

出典と根拠

ORDレコード
ord-aaca21f669b0494ab5bbb28e421cad37
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08426411B2

反応ノート

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