Water → HCID 565576, Verbindung

HRID 611470Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 611470
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1([CH3:19])[C:12]2([C:16](O)=[O:17])[C:13]([CH2:15][CH:9]1[CH2:10][CH2:11]2)=[O:14].O>CCOCC>[CH3:7][C:8]1([CH3:19])[CH:9]2[CH2:10][CH2:11][C:12]1([CH2:16][OH:17])[CH:13]([OH:14])[CH2:15]2

Komponenten

5

Edukt 3

HCID 962WaterHCID 2978887,7-Dimethyl-2-oxobicyclo[2.2.1]heptane-1-carboxylic acidHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 565576HCID 565576, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

To an ice-cooled mixture of lithium aluminum hydride (4 g, 105.4 mmol) in ether was added dropwise a solution of camphorsulfonyl chloride (10 g, 39.88 mmol) and ketopinic acid, prepared as described in Step 1, above. After the addition was complete, the ice bath was removed and the mixture was stirred at ambient temperature for 2 hrs. The mixture was cooled again and wet ether was added cautiously. When the violent reaction subsided, water was added. The mixture was then extracted three times with ethyl acetate. The combined extracts were washed with water and brine and dried over anhydrous magnesium sulfate. Evaporation of the solution gave 4.8 g of a white powder. NMR(δ): 0.90 (s, 3H), 1.20 (s, 3H).

Aufarbeitung

  1. customprepared
  2. additionAfter the addition
  3. customthe ice bath was removed
  4. temperatureThe mixture was cooled again
  5. additionwet ether was added cautiously
  6. customWhen the violent reaction
  7. extractionThe mixture was then extracted three times with ethyl acetate
  8. washThe combined extracts were washed with water and brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customEvaporation of the solution

Quellen und Nachweise

ORD-Eintrag
ord-c228431786e849d9b296ba6763ed91b2
Quelldatensatz
uspto-grants-1999_12
Patentnummer
US06001659

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