Toluene → 1,4-Benzenedicarboxylic acid, 1-methyl ester, potassium salt (1:1)

HRID 1089639

Reaktionsgleichung

[O-]S([O-])(=O)=O.[Ca+2].[C:7]([O:19]C)(=[O:18])[C:8]1[CH:17]=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[CH:10][CH:9]=1.C1(C)C=CC=CC=1.[OH-].[K+:29]>CO>[C:12]([O:14][CH3:15])(=[O:13])[C:11]1[CH:16]=[CH:17][C:8]([C:7]([O-:19])=[O:18])=[CH:9][CH:10]=1.[K+:29]

Komponenten

Reaktionsbedingungen

Temperatur: 67.5 °C

Versuchsvorschrift

To a three-necked 50 ml round bottom flask equipped with a mechanical stirrer, reflux condenser and an addition funnel topped with a drying tube containing indicating Drierite® were added 2.70 gm (0.0139 mole) of dimethyl terephthalate (ex Aldrich Chemical Co.) and 15 ml of toluene. A solution containing 0.76 gm (0.0136 mole) of potassium hydroxide and 10 ml of methanol was added dropwise to the diester solution. The mixture formed an immediate emulsion. The emulsion was heated to 65-70° C. and soon thereafter a precipitate began to form. After 30 minutes the reaction was complete. The mixture was cooled to room temperature and the solid collected on a Buchner funnel. The filter cake was washed several times with warm toluene and ether; thereupon the cake was dried in a vacuum oven at 60° C. The yield was 2.85 gm (96%).

Aufarbeitung

customTo a three-necked 50 ml round bottom flask equipped with a mechanical stirrer
temperaturereflux condenser and an addition funnel
customtopped with a drying tube
additioncontaining
customThe mixture formed an immediate emulsion
customto form
temperatureThe mixture was cooled to room temperature
customthe solid collected on a Buchner funnel
washThe filter cake was washed several times with warm toluene and ether
customthereupon the cake was dried in a vacuum oven at 60° C

Quellen und Nachweise

ORD-Eintrag: ord-8b901168809e47d8a144a20616cc9a20
Quelldatensatz: uspto-grants-1992_01
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05078907

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