Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Oxalic Acid | HCID 971 | — |
| Reactant | HCID 20310599 | HCID 20310599 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 53977657 | HCID 53977657 | — |
| Product | HCID 73676001 | HCID 73676001 | — |
Reaction Steps
2-Cyano-11-(3-dimethylaminopropyl)-11-hydroxy-6,11-dihydro-5H-pyrrolo[2,1-b][3]benzazepine (.62 g.) and 6.2 g. Ni-Al 1:1 alloy powder (BDH Chemicals Ltd., Pool England) in 50 ml. 75% formic acid is refluxed for 1 hr. The dark red suspension is cooled, filtered to remove the insolubles, washed with formic acid and evaporated to dryness. The yield of this red oil is 3.4 g. (57%) and it slowly crystallizes on cooling. The oxalate salt of 2-formyl-11-(3-dimethylaminopropylidene)-6,11-dihydro-5H-pyrrolo[2,1-b][3]-benzazepine is prepared by dissolving the above product in the minimum volume of ethanol and adding dropwise a saturated ethanolic solution of oxalic acid. The resulting crystals are collected by filtration and dried to give 2-formyl-11-(3-dimethylaminopropylidene)-6,11-dihydro-5H-pyrrolo[2,1-b][3]benzazepine oxalate, m.p. 181° C. (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04112112 |
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| Source dataset | uspto-grants-1978_09 |
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| ORD ID | ord-7528d5080d0143ca9383998b20fde4ec |
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| Source note | uspto-grants-1978_09 |
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