Potassium Carbonate → HCID 57909153, Verbindung

HRID 1918434Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1918434
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]2[CH:13]=[C:12]([CH3:14])[CH:11]=[C:10]([CH3:15])[CH:9]=2)[C:3]=1[C:16]([OH:18])=O.C([O-])([O-])=O.[K+].[K+]>S(=O)(=O)(O)O>[CH3:14][C:12]1[C:13]2[C:16](=[O:18])[C:3]3[C:4](=[CH:5][CH:6]=[CH:7][C:2]=3[CH3:1])[C:8]=2[CH:9]=[C:10]([CH3:15])[CH:11]=1

Komponenten

4

Edukt 2

HCID 11430Potassium CarbonateHCID 532252822-(3,5-Dimethylphenyl)-6-methylbenzoic acid

Produkt 1

HCID 57909153HCID 57909153, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

In a 250 ml 1-necked round bottom flask the biphenyl-carboxylic acid 52 (3.0 g, 12.9 mmol) was treated with concentrated sulphuric acid (40 ml) at 0° C. (ice bath). The resulting dark brown solution was stirred for 15 min at 0° C., then for additional 1 h at ambient temperature. The reaction mixture was poured in ice (100 g) whereupon the color changes to a bright yellow. The suspension was neutralized with K2CO3 and extracted with Et2O (3×100 ml). The combined organic phases were washed with brine (75 ml), dried over MgSO4, filtered and the volatiles removed in vacuo to afford 53 (2.8 g, 98%) as yellow crystals. Rf 0.52 (cyclohexane:ethylacetate 10:1). The product was used without any further purification.

Aufarbeitung

  1. waitfor additional 1 h at ambient temperature
  2. extractionextracted with Et2O (3×100 ml)
  3. washThe combined organic phases were washed with brine (75 ml)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe volatiles removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b021fec436f3400bb8e4ca1c5c30ef20
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08618328B2

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