Acetyl chloride → HCID 11349821, Verbindung

HRID 17868Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 17868
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=[O:13])[N:8]([CH3:14])[C:7]([CH:15]1[CH2:20][CH2:19][CH2:18][NH:17][CH2:16]1)=[C:6]2[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(N(CC)C(C)C)(C)C.[C:36](Cl)(=[O:38])[CH3:37].C(=O)(O)[O-].[Na+]>ClCCl>[C:36]([N:17]1[CH2:18][CH2:19][CH2:20][CH:15]([C:7]2[N:8]([CH3:14])[C:9](=[O:13])[C:10]3[C:5]([C:6]=2[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=3)[CH2:16]1)(=[O:38])[CH3:37]

Komponenten

6

Edukt 4

HCID 6367Acetyl chlorideHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 11279492(+/-)-6-Methoxy-2-methyl-4-phenyl-3-piperidin-3-ylisoquinolin-1(2H)-one

Produkt 1

HCID 11349821HCID 11349821, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a dichloromethane (0.100 mL) solution of (±)-6-methoxy-2-methyl-4-phenyl-3-piperidin-3-ylisoquinolin-1(2H)-one (30 mg, 0.086 mmol) and N,N-diisopropylethylamine (0.017 mL, 0.095 mmol) was added acetyl chloride (0.007 mL, 0.095 mmol). After 24 hours saturated sodium bicarbonate and additional dichloromethane were added. The layers were separated and the organic phase dried with anhydrous magnesium sulfate. Evaporation of the solvent in vacuo followed by trituration with ether-EtOAc gave a white solid which was isolated by vacuum filtration to give the titled product. ESI+MS: 391.3 [M+H]+.

Aufarbeitung

  1. customThe layers were separated
  2. dry with materialthe organic phase dried with anhydrous magnesium sulfate
  3. customEvaporation of the solvent in vacuo
  4. customgave a white solid which
  5. customwas isolated by vacuum filtration

Quellen und Nachweise

ORD-Eintrag
ord-272a06a7c288415186946daf41104208
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07741322B2

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