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Benzoyl chloride → 6-Hydroxy-7-benzoyl-1,2,3,4-tetrahydro-1-naphthylacetic acid ethyl ester

HRID 1680281
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1680281
[Cl-].[Al+3].[Cl-].[Cl-].[CH2:5]([O:7][C:8](=[O:22])[CH2:9][CH:10]1[C:19]2[C:14](=[CH:15][C:16]([O:20]C)=[CH:17][CH:18]=2)[CH2:13][CH2:12][CH2:11]1)[CH3:6].[C:23](Cl)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C(Cl)Cl>[CH2:5]([O:7][C:8](=[O:22])[CH2:9][CH:10]1[C:19]2[C:14](=[CH:15][C:16]([OH:20])=[C:17]([C:23](=[O:30])[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:18]=2)[CH2:13][CH2:12][CH2:11]1)[CH3:6]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 7412Benzoyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 13420659Ethyl 2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-1-yl)acetate

Produkt 1

HCID 540031226-Hydroxy-7-benzoyl-1,2,3,4-tetrahydro-1-naphthylacetic acid ethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

26.6 g of finely powdered aluminium chloride are added in portions to a solution of 10 g of 6-methoxy-1,2,3,4-tetrahydro-1-naphthyl-acetic acid ethyl ester in 50 ml of absolute methylene chloride whilst stirring at 5° C., and thereafter 16.9 g of benzoyl chloride are added sufficiently slowly that the reaction solution boils gently under reflux. After completion of the addition, the reaction mixture is allowed to boil for a further 30 minutes and is then allowed to cool to room temperature, after which it is poured onto 300 g of ice. The mixture is extracted with 3 times 100 ml of methylene chloride and the organic phases are washed until neutral, dried over sodium sulphate and evaporated to dryness in vacuo. Chromatography of the evaporation residue on 500 g of silica gel, using methylene chloride as the eluting agent, gives 6-hydroxy-7-benzoyl-1,2,3,4-tetrahydro-1-naphthylacetic acid ethyl ester of boiling point 190° C./0.04 mm Hg.

Aufarbeitung

  1. temperatureunder reflux
  2. additionAfter completion of the addition
  3. temperatureto cool to room temperature
  4. extractionThe mixture is extracted with 3 times 100 ml of methylene chloride
  5. washthe organic phases are washed until neutral,
  6. dry with materialdried over sodium sulphate
  7. customevaporated to dryness in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-781caa7872a74ced886629926304a523
Quelldatensatz
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04272547

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