Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 19420958 | HCID 19420958 | — |
| Catalyst | Platinum oxide (PtO) | HCID 82844 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 19420920 | HCID 19420920 | 53.1% |
Reaction Steps
1.03 g (3.5 mmol) of (RS)-1-(2-azido-propyl)-7-methoxy-4,4-dimethyl-1,4-dihydro-indeno[2,1-c]pyrazole dissolved in 50 ml of anhydrous ethanol were hydrogenated over 100 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 colorless oil obtained was dissolved in 80 ml of anhydrous diethyl ether, filtered and treated while stirring with a solution of 440 mg (3.5 mmol) of fumaric acid in 15 ml of methanol. The mixture was stirred at room temperature for 15 hours and the white crystals were subsequently filtered off. 0.72 g (53%) of (RS)-2-(7-methoxy-4,4-dimethyl-1,4-dihydroindeno[2,1-c]pyrazol-1-yl)-1-methyl-ethylamine fumarate (1:1) with m.p. 178°-180° were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05561150 |
|---|
| Source dataset | uspto-grants-1996_10 |
|---|
| ORD ID | ord-135ed2bda90a43f3bc3128080ebcf57e |
|---|
| Source note | uspto-grants-1996_10 |
|---|