Process for the separation of palladium catalyst from crude reaction mixtures of aryl acetic acids obtained by carbonylation
First Claim
1. A process for the separation of palladium from a crude reaction mixture comprising aryl acetic acids of the general formula wherein Z means phenyl, napht-2-yl, 9H-fluoren-2-yl, substituted carbazol-2-yl, benzoxazol-5-yl, either of which can be substituted with H, C1-C8-alkyl or C1-C8-cycloalkyls optionally substituted with —
- F or —
Cl, C6-C10-aryl optionally substituted with F or Cl, OR4, COR5, —
F, —
Cl; and
pyrrolyl or dehydropyrrolyl or 1-oxo-1,3-dehydro-isoindol-2-yl optionally substituted with F or Cl, OR4, COR5, —
F, —
Cl;
R1 means H or C1-C4-alkyl; and
R2, R3, R4, R5 mean independently of each other;
H, C1-C8 alkyl, C6-C10-aryl optionally substituted with —
F or —
Cl, or thiophenyl;
wherein the crude reaction mixture is obtained by palladium catalyzed carbonylation by adsorption of the palladium on a solid adsorbent, characterized in that the adsorption is carried out in the absence of a reducing agent for palladium and at a temperature, in which the crude reaction mixture is molten.
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Abstract
A process for the separation of palladium from solvent-free at room temperature solid crude reaction mixtures comprising aryl acetic acids of the general formula (I), wherein Z means phenyl, napht-2-yl, 9H-fluoren-2-yl, substituted carbazol-2-yl, benzoxazol-5-yl, either of which can be substituted with H, C1-C8-alkyl optionally cyclic and optionally substituted with —F or —Cl, C6-C10-aryl optionally substituted with F or Cl OR4, COR5, F, —Cl; optionally substituted pyrrolyl or dehydropyrrolyl or 1-oxo-1,3-dehydro-isoindol 2-yl; R1 means H or C1-C4-alkyl; R2, R3, R4, R5 mean independently of each other H, C1-C8 alkyl, C6-C10-aryl optionally substituted with —F or Cl, or thiophenyl; which crude mixture is obtained by palladium catalyzed carbonylation, by adsorption of the palladium on solid adsorbents, characterized in that the adsorption is carried out in the absence of a reducing agent for palladium and at a temperature, where the crude reaction mixture is molten.
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Citations
20 Claims
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1. A process for the separation of palladium from a crude reaction mixture comprising aryl acetic acids of the general formula
wherein Z means phenyl, napht-2-yl, 9H-fluoren-2-yl, substituted carbazol-2-yl, benzoxazol-5-yl, either of which can be substituted with H, C1-C8-alkyl or C1-C8-cycloalkyls optionally substituted with — - F or —
Cl, C6-C10-aryl optionally substituted with F or Cl, OR4, COR5, —
F, —
Cl; and
pyrrolyl or dehydropyrrolyl or 1-oxo-1,3-dehydro-isoindol-2-yl optionally substituted with F or Cl, OR4, COR5, —
F, —
Cl;
R1 means H or C1-C4-alkyl; and
R2, R3, R4, R5 mean independently of each other;
H, C1-C8 alkyl, C6-C10-aryl optionally substituted with —
F or —
Cl, or thiophenyl;
wherein the crude reaction mixture is obtained by palladium catalyzed carbonylation by adsorption of the palladium on a solid adsorbent, characterized in that the adsorption is carried out in the absence of a reducing agent for palladium and at a temperature, in which the crude reaction mixture is molten. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16)
- F or —
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17. A process for the separation of palladium from a crude reaction mixture containing ibuprofen, wherein the crude reaction mixture is obtained by palladium catalyzed carbonylation by adsorption of the palladium on a solid adsorbent, characterized in that the adsorption is carried out in the absence of a reducing agent for palladium and at a temperature of 40°
- C. to 200°
C. - View Dependent Claims (18, 19, 20)
- C. to 200°
Specification