Methyl iodide → HCID 178501284, Verbindung

HRID 217228Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 217228
[OH:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([C:8]([OH:10])=[O:9])[CH2:4][CH2:3]1.[C:11]([O-])([O-])=O.[K+].[K+].IC>CN(C=O)C.CCOC(C)=O>[CH3:11][O:9][C:8]([C@H:5]1[CH2:6][CH2:7][C@@H:2]([OH:1])[CH2:3][CH2:4]1)=[O:10]

Komponenten

6

Edukt 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178525780HCID 178525780, Verbindung

Produkt 1

HCID 178501284HCID 178501284, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of trans-4-hydroxycyclohexanecarboxylic acid (5.0 mmol, 721 mg), K2CO3 (15.0 mmol, 2.07 g) in DMF (17 mL) is added iodomethane (6.0 mmol, 0.374 mL). After stirring for 2 h, the mixture is diluted with EtOAc. The mixture is washed with H2O and brine, dried over Na2SO4 and concentrated. The residue is used to next reaction without further purification (643 mg, 81%); ESI-MS m/z: 159 [M+1]+, Retention time 1.34 min. (condition A).

Aufarbeitung

  1. washThe mixture is washed with H2O and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. customThe residue is used to next reaction without further purification (643 mg, 81%)

Quellen und Nachweise

ORD-Eintrag
ord-d80ff8c0710145e385dfecaf90ac252b
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08193349B2

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