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Acetic Anhydride → N-[2-(1-methyl-8,9-dihydro-7H-cyclopenta[c]pyrazolo[1,5-a]pyridin-9-yl)ethyl]acetamide

HRID 887806
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 887806
[NH2:1][CH2:2][CH2:3][CH:4]1[C:8]2[C:9]3[N:10]([N:13]=[CH:14][C:15]=3[C:16](OCC)=O)[CH:11]=[CH:12][C:7]=2[CH2:6][CH2:5]1.C1(C)C=CC=CC=1.[H-].C([Al+]CC(C)C)C(C)C.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+].C(N(CC)CC)C.[C:62](OC(=O)C)(=[O:64])[CH3:63]>O1CCCC1.O>[CH3:16][C:15]1[CH:14]=[N:13][N:10]2[CH:11]=[CH:12][C:7]3[CH2:6][CH2:5][CH:4]([CH2:3][CH2:2][NH:1][C:62](=[O:64])[CH3:63])[C:8]=3[C:9]=12
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 62649Sodium sulfate decahydrateHCID 59145841ethyl 9-(2-aminoethyl)-8,9-dihydro-7H-cyclopenta[c]pyrazolo[1,5-a]pyridine-1-carboxylateHCID 86583787Diisobutylaluminumhydride toluene

Produkt 1

HCID 59145930
N-[2-(1-methyl-8,9-dihydro-7H-cyclopenta[c]pyrazolo[1,5-a]pyridin-9-yl)ethyl]acetamide
Ausbeute 17,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a solution of ethyl 9-(2-aminoethyl)-8,9-dihydro-7H-cyclopenta[c]pyrazolo[1,5-a]pyridine-1-carboxylate (45.0 mg, 0.165 mmol) in tetrahydrofuran (1.7 mL) was added 1.5M diisobutylaluminum hydride toluene solution (1.3 mL, 1.95 mmol) at room temperature, and the mixture was stirred for 3 hr. Sodium sulfate decahydrate (1.3 g) was added, and the mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. To a mixture of the residue and triethylamine (34.5 μL, 0.248 mmol) in tetrahydrofuran (1.7 mL) was added acetic anhydride (23.4 μL, 0.248 mmol) under ice-cooling, and the mixture was stirred at room temperature for 15 min. Water (50 μL) was added, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→5/95) and recrystallization (ethyl acetate/diisopropyl ether) to give the title compound (7.3 mg, yield 17%).

Aufarbeitung

  1. filtrationthe mixture was filtered through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. temperaturecooling
  4. stirringthe mixture was stirred at room temperature for 15 min
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→5/95) and recrystallization (ethyl acetate/diisopropyl ether)

Quellen und Nachweise

ORD-Eintrag
ord-527bec76b41c4510b91b4f3f6bbe65f0
Quelldatensatz
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08247429B2

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