Water → HCID 20384467, Verbindung

HRID 838790Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 838790
[CH3:1][CH:2]([C:4]([CH3:8])([OH:7])[CH2:5][CH3:6])[CH3:3].C[Li].Cl[C:12]([O:14][CH2:15][C:16](=[CH2:18])[CH3:17])=[O:13].O>O1CCCC1.C(OCC)C>[C:12](=[O:13])([O:14][CH2:15][C:16](=[CH2:17])[CH3:18])[O:7][C:4]([CH3:8])([CH2:5][CH3:6])[CH:2]([CH3:3])[CH3:1]

Komponenten

7

Edukt 4

HCID 962WaterHCID 116852,3-Dimethylpentan-3-olHCID 170604Carbonochloridic acid, 2-methyl-2-propen-1-yl esterHCID 178418348HCID 178418348, Verbindung

Produkt 1

HCID 20384467HCID 20384467, VerbindungAusbeute 94,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of 13.94 grams (0.12 mole) of 2,3-dimethylpentan-3-ol in 75 milliliters of anhydrous tetrahydrofuran at 0° C under a nitrogen atmosphere was added with stirring one equivalent of methyllithium in diethyl ether. Then 19.31 grams (0.14 mole) of methallyl chloroformate in 25 milliliters of anhydrous tetrahydrofuran was added. During additions the temperature was maintained at 0° C. Cooling was discontinued and the reaction mixture was stirred for about 18 hours. The reaction mixture was poured into water, and then extracted with ether. The ether layer was separated and washed with water, and then dried over magnesium sulfate. Removal of solvent under reduced pressure yielded 24.32 grams (94.6%) of a yellow oil. A pure sample was obtained by vacuum distillation (Fraction 2).

Aufarbeitung

  1. temperatureCooling
  2. extractionextracted with ether
  3. customThe ether layer was separated
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. customRemoval of solvent under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-627e7d89d7424008841fee1e77b588c0
Quelldatensatz
uspto-grants-1978_06
Patentnummer
US04092988

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