HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 19956226, compound → HCID 19956218, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 19956226 | HCID 19956226 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 19956218 | HCID 19956218 | 28% |
Reaction Steps
A solution of 8.5 g (30.9 mmol) of N-[5-chloro-2-(pyrrol-1-yl)benzoyl]pyrrolidine (Preparation 23) in 70 ml of phosphorus oxychloride is heated at 100° C. for 35 minutes. After cooling, the precipitate formed is isolated by filtration, washed with petroleum ether to remove excess phosphorus oxychloride, and then redissolved in 30 ml of water. The aqueous solution is rendered alkaline by the dropwise addition of 10% sodium hydroxide solution and the precipitate formed is filtered and extracted with 100 ml of ethyl acetate. The organic phase is washed with water, dried over magnesium sulfate, rendered colourless with animal charcoal and concentrated under reduced pressure to yield 1.76 g of the title product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05627203 |
| Source dataset | uspto-grants-1997_05 |
| ORD ID | ord-41a72cd335f742259104f62051699aae |
| Source note | uspto-grants-1997_05 |