Hydrochloric Acid → HCID 10630901, Verbindung

HRID 19372

Reaktionsgleichung

Reaktionsgleichung von HRID 19372
[CH3:1][Mg]Br.COC(=O)[CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([OH:14])[CH:9]=1.C([O:19][CH2:20][CH3:21])(=O)C.Cl>O1CCCC1.O>[OH:14][C:10]([CH3:11])([CH3:1])[CH2:9][C:8]1[CH:7]=[C:20]([OH:19])[CH:21]=[CH:12][CH:13]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 39129Methyl 3-HydroxyphenylacetateHCID 178418573HCID 178418573, Verbindung

Produkt 1

HCID 10630901HCID 10630901, VerbindungAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a solution of methyl magnesium bromide (3 M, 12 mL, 36.06 mmol) cooled to 0° C. was added tetrahydrofuran (10 mL) and (3-hydroxy-phenyl)-acetic acid methyl ester (1 g, 6.01 mmol) as a solution in tetrahydrofuran (5 mL). The resulting mixture was warmed to room temperature stirred for 30 min and then poured carefully into a biphasic mixture of ethyl acetate and water. The water layer was made acidic (pH=1) with 1N aqueous hydrochloric acid and extracted twice with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo which afforded 3-(2-hydroxy-2-methyl-propyl)-phenol (1 g, 100%) as a white solid.

Aufarbeitung

  1. extractionextracted twice with ethyl acetate
  2. dry with materialThe combined organic phases were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo which

Quellen und Nachweise

ORD-Eintrag
ord-deeeda5aef424b77a2cee8a8fc33472c
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07741327B2

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