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Phenothiazine → Diethyl allylphosphonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenothiazine | HCID 7108 | — |
| 反応物 | Allyl chloride | HCID 7850 | — |
| 反応物 | Triethyl phosphite | HCID 31215 | — |
| 触媒 | Cobalt | HCID 104730 | — |
| 生成物 | Diethyl allylphosphonate | HCID 573014 | — |
反応手順
166 parts of triethyl phosphite are heated for 1 hour to 140° C in a nitrogen atmosphere with 2 parts of highly active Raney cobalt (Ra-Co-Lu). A mixture of 1 part of phenothiazine and 80 parts of allyl chloride is then added dropwise at 140° C. Once the reaction has started, the temperature may be lowered to 120° C. After 5.5 hours, 63 parts of ethyl chloride have distilled off and the mixture is deep blue in colour. Fractional distillation gives 135 parts of allyl phosphonic acid diethyl ester, corresponding to 76% of the theoretical yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04017564 |
| 出典データセット | uspto-grants-1977_04 |
| ORD ID | ord-d23f6875737846dd9075b4bb91fd9f56 |
| 出典メモ | uspto-grants-1977_04 |