Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Magnesium Acetate | HCID 8896 | — |
| Reactant | 2,4-Diaminopropoxybenzene | HCID 153693 | — |
| Reactant | 2,4-Bis-acetylamino-1-n-propoxybenzene | HCID 56690812 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 20267383 | HCID 20267383 | 88.9% |
Reaction Steps
208 parts of dried crude 6-n-propoxy-3-acetylamino-aniline obtained according to Example 7 of European Pat. No. 0,011,048 (containing, in addition to 190.3 parts of target product, 8.8 parts of 2,4-bis-acetylamino-1-n-propoxybenzene and 3.5 parts of 2,4-diamino-1-n-propoxybenzene, as well as small amounts of magnesium acetate and oxidative decomposition products) are dissolved in 300 parts of ethanol at 50° C., with stirring, and, after the solution has been cooled to 25° C., 170 parts of 48% strength hydrobromic acid are added dropwise in the course of 1.5 hours. The precipitate which has separated out is filtered off with suction at 0°-5° C., washed with two portions of 60 parts of ethanol and dried in vacuo. 257.1 parts of 6-n-propoxy-3-acetylamino-aniline hydrobromide (no impurities detectable by HPLC, purity by diazotization: 99.4%) are obtained, which corresponds to a yield of 88.9% of theory (based on the crude feed product) or 97.2% of theory (based on the target product contained therein).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04540815 |
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| Source dataset | uspto-grants-1985_09 |
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| ORD ID | ord-bdd1d955f3904ae3b66064748f09f04a |
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| Source note | uspto-grants-1985_09 |
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