HuagongsheHuagongshe Chemistry Print Report · For research reference only
Catechol → HCID 12957960, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Catechol | HCID 289 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Phenylphosphonic dichloride | HCID 69990 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 12957960 | HCID 12957960 | 94.4% |
Reaction Steps
To a solution of 3.11 g of phenylphosphonic acid dichloride in 10 ml of ether were added 1.76 g of pyrocatechol and 20 ml of ether. The resulting solution was cooled to -25° C. to -28° C. and a solution of 3.23 g of triethylamine in 10 ml of ether was added dropwise thereto with stirring over 8 minutes. Thereafter, the reaction mixture was allowed to return to room temperature (20°-25° C.), and the precipitate was filtered off under nitrogen atmosphere and washed with 30 ml of ether. The filtrate and washings were combined and the ether was distilled off under reduced pressure to give 3.46 g (94.4% yield) of 2-phenyl-2-oxo-1,3,2-benzodioxaphosphole as a colorless oil. Upon standing in a refrigerator overnight, it crystallized.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04801703 |
| Source dataset | uspto-grants-1989_01 |
| ORD ID | ord-49c8f63fd98f41d3b40df04dd7e524da |
| Source note | uspto-grants-1989_01 |