Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 4,5-Dimethyl-1,2-phenylenediamine | HCID 76635 | — |
| Reactant | 2-Chloro-4,6-dimethylnicotinic acid | HCID 591127 | — |
| Solvent | Sulfolane | HCID 31347 | — |
| Product | HCID 20393029 | HCID 20393029 | — |
Reaction Steps
A mixture consisting of 52.0 gm of 2-chloro-4,6-dimethyl-nicotinic acid, 38.0 gm of 4,5-dimethyl-o-phenylenediamine and 150 ml of sulfolane was heated on an oil bath at 220° C. After 45 minutes the mixture was allowed to cool to 100° C. and was then poured over ice. After neutralization with ammonia and standing for several hours the precipitate which had formed was suction-filtered off and admixed with dilute acetic acid. The mixture was suction-filtered after one hour, and the filter cake was recrystallized from aqueous 80% acetic acid, yielding 34% of theory of the compound named in the heading, which had a melting point of 264°-268° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04167570 |
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| Source dataset | uspto-grants-1979_09 |
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| ORD ID | ord-9547794dcb7d42eda3c9e4a7a9e90984 |
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| Source note | uspto-grants-1979_09 |
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