Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | N-Ethylaniline | HCID 7670 | — |
| Reactant | Triphenylphosphine dichloride | HCID 260420 | — |
| Reactant | 5-Chloro-4-hydroxy-1-methyl-2-oxo-1,2-dihydroquinoline-3-carboxylic acid | HCID 54720227 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | Laquinimod | HCID 54677946 | 92.1% |
Reaction Steps
N-Ethyl aniline (5.2 gm) was taken in chloroform (100 ml) and stirred for 10 minutes at 25-30° C. under nitrogen atmosphere. The resulting mass was followed by the addition of dichlorotriphenyl phosphorane (26.6 gm) at 25-30° C. and the reaction mixture was stirred for 15 minutes. 1,2-Dihydro-4-hydroxy-5-chloro-1-methyl-2-oxo-quinoline-3-carboxylic acid (10 gm) was added to the resulting mass at 25-30° C. followed by heating to reflux (40-45° C.) and then stirred for 3 hours at reflux. Chloroform was distilled out from the reaction mass under vacuum at below 55° C. The resulting residue was cooled to 25-30° C., followed by the addition of ethyl acetate (50 ml) and water (50 ml) at 25-30° C. and the resulting mixture was stirred for 30 minutes at 25-30° C. The separated solid was filtered, washed with water and then dried to yield 12.95 gm of laquinimod (HPLC purity: 99.24%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08552194B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-07248633b2a645f0a7b1ea58d61966de |
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| Source note | uspto-grants-2013_10 |
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