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Phenyl phosphorus dichloride → O-(2,6-Di-tert-butyl-4-methylphenyl) phenylphosphonochloridite
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenyl phosphorus dichloride | HCID 12573 | — |
| 反応物 | 2,6-Di-tert-butyl-4-methylphenol | HCID 31404 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | O-(2,6-Di-tert-butyl-4-methylphenyl) phenylphosphonochloridite | HCID 53944288 | — |
反応手順
To a solution of 110 grams of 2,6-di-tert-butyl-p-cresol in 252 grams of triethylamine was added at 25°-26° C. over a 15-minute period 89.5 grams of dichlorophenylphosphine. The reaction mixture was heated for 31 hours at 95°-97° C. The excess triethylamine solvent was then removed by distillation under vacuum, the resulting residue was triturated with 200 ml of dry benzene, and the white crystalline solid triethylamine hydrochloride was separated by filtration. The desired product named above was isolated from the filtrate by distillation of the benzene under vacuum and crystallization of the residue from acetonitrile. The product was obtained as white crystals melting at 103°-106° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04233207 |
| 出典データセット | uspto-grants-1980_11 |
| ORD ID | ord-303f5b93ae484918862c034fb97dfa07 |
| 出典メモ | uspto-grants-1980_11 |