Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178423777 | HCID 178423777 | — |
| Product | 1422469-43-9 | HCID 79857819 | 78.8% |
Reaction Steps
Phosphorous oxychloride (1.9 mL, 24 mmol) was added to 2-hydroxy-7,7-dimethyl-6,7-dihydro-5H-cyclopenta[b]pyridine-3-carbonitrile (0.8 g, 4.3 mmol), obtained in step-1, at 0° C. over a period of about 10 min. The mixture was warmed to a temperature of about 20-35° C. and was heated further to about 80° C. The mixture was stirred at about 80° C. for about 18 h. The reaction mixture was cooled to a temperature of about 20-35° C. and then was poured into crushed ice. The solid which separated out was filtered off and dried under reduced pressure to get 2-chloro-7,7-dimethyl-6,7-dihydro-5H-cyclopenta[b]pyridine-3-carbonitrile (0.7 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09351969B2 |
|---|
| Source dataset | uspto-grants-2016_05 |
|---|
| ORD ID | ord-6f8f50bec4284e4b9017e2e41844407b |
|---|
| Source note | uspto-grants-2016_05 |
|---|