Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 19420927 | HCID 19420927 | — |
| Catalyst | Platinum oxide (PtO) | HCID 82844 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 19420947 | HCID 19420947 | 83% |
Reaction Steps
1.66 g (5.82 mmol) of (RS)-1-(2-azido-propyl)-7-fluoro-4,4-dimethyl-1,4-dihydro-indeno[2,1-c]pyrazole dissolved in 80 ml of anhydrous ethanol were hydrogenated over 160 mg of platinum oxide for 1.5 hours. The catalyst was subsequently filtered off, rinsed with ethanol and the solvent was removed in a vacuum. The yellow oil obtained was dissolved in 80 ml of anhydrous diethyl ether, filtered and treated while stirring with a solution of 676 mg (5.82 mmol) of fumaric acid in 10 ml of methanol. The mixture was stirred at room temperature for 15 hours and the white crystals were subsequently filtered off. 1.81 g (83%) of (RS)-2-(7-fluoro-4,4-dimethyl-1,4-dihydroindeno[2,1-c]pyrazol-1-yl)- 1-methyl-ethylamine fumarate (1:1) with m.p. 144°-146° were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05561150 |
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| Source dataset | uspto-grants-1996_10 |
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| ORD ID | ord-5b6d8837ff1e4f3baa4091664e3f7d18 |
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| Source note | uspto-grants-1996_10 |
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