Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 53920515 | HCID 53920515 | — |
| Catalyst | Palladium Chloride | HCID 24290 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22749253 | HCID 22749253 | 83.4% |
Reaction Steps
5 g of N-carbethoxy acetyl N-methyl 4-methoxy 2-nitro aniline are dissolved in 50 c.c. of hot ethanol. After cooling, 15 c.c. of water and 3 c.c. of a 2% solution of palladium chloride are added. Then 5 c.c. of a 20% aqueous solution of sodium borohydride are introduced, while cooling. This is agitated for thirty minutes, without allowing the temperature to exceed 40° C. Then, the excess of reagent is decomposed by acidifying to pH = 2 with hydrochloric acid. After cessation of the gaseous emission, the medium is filtered then neutralised with addition of ammonium hydroxide, N-carbethoxy acetyl N-methyl 4-methoxy o-phenylene diamine precipitates. The precipitate is filtered, washed with water, filtered with suction and dried. Thus, there are obtained 3.75 g of N-carbethoxy acetyl N-methyl 4-methoxy o-phenylene diamine, which is purified by recrystallization in ethanol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04001408 |
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| Source dataset | uspto-grants-1977_01 |
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| ORD ID | ord-b6d52664edd948da82aea09f8e9d919b |
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| Source note | uspto-grants-1977_01 |
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