Water → HCID 58097238, Verbindung

HRID 1500109Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1500109
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=[O:8])=[CH:5][CH:4]=1.ClC[C@@H:13]1[CH2:17][O:16][C:15]([CH3:19])([CH3:18])[O:14]1.C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[CH3:18][C:15]1([CH3:19])[O:16][C@H:17]([CH2:1][O:2][C:3]2[CH:10]=[CH:9][C:6]([CH:7]=[O:8])=[CH:5][CH:4]=2)[CH2:13][O:14]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 312444-MethoxybenzaldehydeHCID 6930483(S)-4-Chloromethyl-2,2-dimethyl-1,3-dioxolane

Produkt 1

HCID 58097238HCID 58097238, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

2 g (16.38 mmol) of p-methoxybenzaldehyde together with 3.7 g (24.57 mmol) of (4S)-4-(chloromethyl)-2,2-dimethyl-1,3-dioxolane and 15.8 g (114.64 mmol) of potassium carbonate are stirred in 10 ml of DMF at 130° C. overnight. The mixture is then added to water and extracted with methylene chloride. The organic phase is washed with saturated aqueous sodium chloride solution, dried over sodium sulphate and concentrated. The residue is purified on a silica gel column (mobile phase: cyclohexane/ethyl acetate 5:1). This gives 2.42 g (61% of theory) of the target compound.

Aufarbeitung

  1. extractionextracted with methylene chloride
  2. washThe organic phase is washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated
  5. customThe residue is purified on a silica gel column (mobile phase: cyclohexane/ethyl acetate 5:1)

Quellen und Nachweise

ORD-Eintrag
ord-4c2f643a062a4c88b766f04cae0bb3ed
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09205077B2

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