HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 135621732, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | HCID 23084651 | HCID 23084651 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 135621732 | HCID 135621732 | 146% |
Reaction Steps
A solution of 5-amino-4-(4-fluorophenyl)-1,3-dimethylpyrazole (20.0 g) and pyridine (23.6 mL) in dichloromethane (150 mL) was added dropwise over 30 min to a solution of triphosgene (11.6 g) in dichloromethane (100 mL) under ice-cooling, and the mixture was stirred at room temperature for 2 hrs. The reaction solution was added dropwise to a solution of aluminum chloride (97.5 g) in dichloromethane under ice-cooling, and the mixture was stirred at room temperature for 2 days. After the completion of the reaction, the reaction solution was poured into ice-water. The precipitated crystals were collected by filtration and washed with water to give 7-fluoro-1,3-dimethyl-3H-pyrazolo[3,4-c]isoquinolin-5(4H)-one (13.2 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07501412B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-b0de85afc5504ce0a68ce8a449cd283a |
| Source note | uspto-grants-2009_03 |