HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 11681702, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Bis(2-oxo-3-oxazolidinyl)phosphinic chloride | HCID 152842 | — |
| Reactant | 1,3-dimethyl-1H-pyrazole-4-carboxylic acid | HCID 1273304 | — |
| Reactant | 3'-chloro-4'-fluoro-2-aminobiphenyl | HCID 11600999 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11681702 | HCID 11681702 | — |
Reaction Steps
At room temperature, 0.47 g of 3′-chloro-4′-fluoro-2-aminobiphenyl and 0.82 g of bis(2-oxo-3-oxazolidinyl)phosphoryl chloride were added to a solution of 0.30 g of 1,3-dimethyl-1H-pyrazole-4-carboxylic acid and 0.43 g of triethylamine in 30 ml of dichloromethane. The mixture was stirred at room temperature for 12 hours. The mixture was then washed successively twice with dilute hydrochloric acid, twice with aqueous sodium bicarbonate solution and once with water. The organic phase was dried and concentrated. The crude product was purified by silica gel column chromatography using cyclohexane/methyl tert-butyl ether 1:2. This gave 0.56 g of the desired product as white crystals of m.p. 177-180° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08008232B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-1d335c10f31e4aeb991df57042f4ce6d |
| Source note | uspto-grants-2011_08 |