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Hydrochloric Acid → Ethyl 6-acetyl-8-(benzyloxy)-2-(4-fluorobenzyl)-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]-pyrazine-7-carboxylate

HRID 494085
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 494085
[CH2:1]([O:8][C:9]1[C:10]([C:28]([O:30][CH2:31][CH3:32])=[O:29])=[C:11](Br)[N:12]2[CH2:17][CH2:16][N:15]([CH2:18][C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=3)[C:14](=[O:26])[C:13]=12)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN(C1CCCCC1)C1CCCCC1.[CH:47]([O:49]CCCC)=[CH2:48].C(P(C(C)(C)C)C(C)(C)C)(C)(C)C.Cl>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:47]([C:11]1[N:12]2[CH2:17][CH2:16][N:15]([CH2:18][C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=3)[C:14](=[O:26])[C:13]2=[C:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:10]=1[C:28]([O:30][CH2:31][CH3:32])=[O:29])(=[O:49])[CH3:48]
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Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 8108Butyl vinyl etherHCID 24210N-Methyl dicyclohexylamineHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 68864116Ethyl 8-(benzyloxy)-6-bromo-2-(4-fluorobenzyl)-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]-pyrazine-7-carboxylate

Produkt 1

HCID 68865319
Ethyl 6-acetyl-8-(benzyloxy)-2-(4-fluorobenzyl)-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]-pyrazine-7-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysatorHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of ethyl 8-(benzyloxy)-6-bromo-2-(4-fluorobenzyl)-1-oxo-1,2,3,4-tetrahydropyrrolo[1,2-a]-pyrazine-7-carboxylate (0.32 g, 0.64 mmol) and N-methyldicyclohexylamine (0.20 mL, 0.96 mmol) in dioxane (1 mL) was purged with nitrogen for 5 minutes, n-butyl vinyl ether (0.83 mL, 6.4 mmol), tris(dibenzylidene-acetone)dipalladium (0.12 g, 0.13 mmol), and tri-tert-butylphosphine (0.065 g, 0.32 mmol) were added. After stirring at room temperature for 2 days, the reaction mixture was treated with 1 N HCl and stirred at room temperature overnight. The reaction mixture was partitioned between chloroform and brine. The organic extract was dried over sodium sulfate, filtered and concentrated. The residue was subjected to column chromatography on silica gel eluted with a hexanes and ethyl acetate gradient to provide titled product.

Aufarbeitung

  1. stirringstirred at room temperature overnight
  2. customThe reaction mixture was partitioned between chloroform and brine
  3. extractionThe organic extract
  4. dry with materialwas dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. washeluted with a hexanes and ethyl acetate gradient

Quellen und Nachweise

ORD-Eintrag
ord-1dfb6bfd4043417da6b589cd41374b83
Quelldatensatz
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07538112B2

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