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Dimethylamine → N,N-dimethyl-2-(1,4-dioxaspiro[4.5]decan-8-yl)acetamide

HRID 243566
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 243566
C[CH2:2][N:3](CC)[CH2:4]C.[CH3:8][N:9](C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)[CH3:10].[B-](F)(F)(F)F.[O:30]1[C:34]2([CH2:39][CH2:38][CH:37]([CH2:40][C:41]([OH:43])=O)[CH2:36][CH2:35]2)[O:33][CH2:32][CH2:31]1.CNC>CN(C=O)C.C1COCC1>[CH3:2][N:3]([CH3:4])[C:41](=[O:43])[CH2:40][CH:37]1[CH2:38][CH2:39][C:34]2([O:33][CH2:32][CH2:31][O:30]2)[CH2:35][CH2:36]1.[CH3:8][N:9]([CH3:10])[C:41](=[O:43])[CH2:40][CH:37]1[CH2:38][CH2:39][C:34](=[O:33])[CH2:35][CH2:36]1
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Komponenten

8

Edukt 4

HCID 674DimethylamineHCID 8471TriethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 151011212-(1,4-Dioxaspiro(4.5)decan-8-yl)acetic acid

Produkt 2

HCID 59442805N,N-dimethyl-2-(1,4-dioxaspiro[4.5]decan-8-yl)acetamide
HCID 59442836
N,N-dimethyl-2-(4-oxocyclohexyl)acetamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

NEt3 (2.0 ml) and TBTU (2.56 g) are added to a solution of 2-(1,4-dioxaspiro[4.5]decan-8-yl)acetic acid (1.45 g; see J. Med. Chem. 1998, 41(5), 760) in DMF (50 ml) and the mixture is stirred for 30 min. 2 M Dimethylamine in THF (7.24 ml) is added. The reaction mixture is stirred for one hour and the solvent is removed under reduced pressure. The residue is dissolved in EtOAc and washed with water and aqueous citric acid (10%, 2×). The organic layer is dried (Na2SO4) and filtered, and the solvent is removed under reduced pressure. The crude product is purified using reverse phase HPLC (Varian C18 Microsorb) eluting with a gradient of 10-100% acetonitrile in water containing 0.2% trifluoroacetic acid to give N,N-dimethyl-2-(1,4-dioxaspiro[4.5]decan-8-yl)acetamide (400 mg) and N,N-dimethyl-2-(4-oxocyclohexyl)acetamide (420 mg).

Aufarbeitung

  1. stirringThe reaction mixture is stirred for one hour
  2. customthe solvent is removed under reduced pressure
  3. dissolutionThe residue is dissolved in EtOAc
  4. washwashed with water and aqueous citric acid (10%, 2×)
  5. dry with materialThe organic layer is dried (Na2SO4)
  6. filtrationfiltered
  7. customthe solvent is removed under reduced pressure
  8. customThe crude product is purified
  9. washeluting with a gradient of 10-100% acetonitrile in water containing 0.2% trifluoroacetic acid

Quellen und Nachweise

ORD-Eintrag
ord-5f3c4ec7742b428bbae9689e0624cbbe
Quelldatensatz
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08653262B2

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