Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 21483887 | HCID 21483887 | — |
| Catalyst | chromium (VI) trioxide | HCID 10219390 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Propionic Acid | HCID 1032 | — |
| Product | HCID 14257701 | HCID 14257701 | — |
Reaction Steps
Chromium trioxide (28 g., 0.028 mole) in 83% acetic acid (12 ml.) is added slowly at 0° C. to a stirred solution of 5,6-dichloro-7-methoxytetralin (4 g., 0.073 mole) in a mixture of acetic acid (90 ml.) and propionic acid (20 ml.). The resulting dark mixture then is kept for 20 hours at 20°-25° C. The resulting dark green solution is poured into a mixture of water (900 ml.) and 96% H2SO4 (10 ml.). The mixture is heated to 70° C., cooled to 0° C. and the precipitate is collected, washed with water, and dried. The dried product is sublimed twice at 100° C. at ca. 0.5 mm. and then crystallized from methanol to obtain 6-methoxy-7,8-dichloro-1-tetralone (1 g.), melting point 132°-132.5° C. The identity of the product is established by proton magnetic resonance (pmr).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04003927 |
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| Source dataset | uspto-grants-1977_01 |
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| ORD ID | ord-905000e52ae447c8a5ac18ed5634bd5f |
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| Source note | uspto-grants-1977_01 |
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