Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 90060-20-1 | HCID 6918482 | — |
| Reactant | HCID 19352269 | HCID 19352269 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19352272 | HCID 19352272 | — |
Reaction Steps
50 g of 2-methoxycarbonylamino-5,6-dimethoxy-1-tetralone are dissolved in 500 ml of methanol in a 1000 ml flask, with stirring, 20 g of 5% Pd/C are added, then the whole is placed into an autoclave (Hastelloy) under hydrogen atmosphere at 80° C. and a pressure of 25 atm. for about 6 hours with stirring, after that the mixture is left to cool to about 30° C. in autoclave. The mixture is filtered through Celite and the filtrate is evaporated to dryness under vacuum. The resulting white solid is triturated in 400 ml of n-hexane at 60° C., then is left to cool to about 30° C. with stirring, filtered and dried under vacuum at 60 ° C., to obtain a whitish solid. Yield: 40.6 g, 85.5% (moles), 81.2% (weight); T.L.C. Methylene chloride 95-Methanol 5; Rf=0.76; M.p.=108.7°-111.4 ° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05710336 |
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| Source dataset | uspto-grants-1998_01 |
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| ORD ID | ord-060cf77c801f4c2b9ab5e12da8b48f29 |
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| Source note | uspto-grants-1998_01 |
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