Water → HCID 13086534, Verbindung

HRID 2416984Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2416984
[CH3:1][C:2]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][C:4]([OH:12])([CH2:5]3)[CH2:3]1)[CH2:9]2.[C:13](OC(=O)C)(=[O:15])[CH3:14].S(=O)(=O)(O)O.O.C(=O)(O)[O-].[Na+]>CCCCCCC.C1CCCCC1.CCOCC>[C:13]([O:12][C:4]12[CH2:5][CH:6]3[CH2:7][CH:8]([CH2:9][C:2]([CH3:1])([CH2:11]3)[CH2:3]1)[CH2:10]2)(=[O:15])[CH3:14]

Komponenten

9

Edukt 5

HCID 962WaterHCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 40715573-Methyl-1-adamantanol

Produkt 1

HCID 13086534HCID 13086534, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 3283Diethyl EtherLösungsmittelHCID 8078CyclohexaneLösungsmittelHCID 8900HeptaneLösungsmittel

Versuchsvorschrift

121 mg (0.728 mmoles) of 3-methyl-1-adamantanol are dissolved in 0.2 mL n-heptane and 0.2 mL cyclohexane. A mixture of 0.2 mL (2.25 mmoles) of acetic anhydride and 2 microliters (0.036 mmoles) of concentrated sulfuric acid is added, and the mixture is at ambient temperature for 20.5 hours. The solution is dissolved in 10 L of ether and extracted with 10 mL of water. The aqueous layer is extracted with 10 mL ether. The ether layers are combined, extracted with 2×mL of water followed by 40 mL of aqueous sodium bicarbonate (10 g/liter), dried over magnesium sulfate, and stripped of solvent in vacuo. The product is a colorless oil with Rf 0.55 (silica: eluant hexane 75%, ethyl acetate 25%).

Aufarbeitung

  1. additionis added
  2. extractionextracted with 10 mL of water
  3. extractionThe aqueous layer is extracted with 10 mL ether
  4. dry with materialdried over magnesium sulfate

Quellen und Nachweise

ORD-Eintrag
ord-23dee9fbdebb4e60a3d63ced5fa5ffbe
Quelldatensatz
uspto-grants-2004_11
Patentnummer
US06825226B2

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