HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formic Acid → Olopatadine impurity 147
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | 2-Cyano-6,11-dihydro-11-oxodibenz[b,e]oxepin | HCID 12446825 | — |
| Catalyst | Nickel | HCID 935 | — |
| Product | Olopatadine impurity 147 | HCID 12446833 | — |
Reaction Steps
Heat a mixture of 5.0 gm. of 2-cyano-6.11-dihydro-11-oxodibenz[b,e]oxepin and 4.0 gm. of Raney nickel alloy in 60 ml. of 75% (v/v) aqueous formic acid at reflux for 1.5 hours. Cool to room temperature and filter. Concentrate to small volume and extract with methylene chloride. Wash the extract with water and with 1 N sodium bicarbonate until neutral. Dry the neutral extract over sodium sulfate and concentrate to dryness to obtain the title product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04282365 |
| Source dataset | uspto-grants-1981_08 |
| ORD ID | ord-2a8e7d02ece34d5786073bf50b2ddd3f |
| Source note | uspto-grants-1981_08 |