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Phenothiazine → Methallyl phosphonic acid diisopropyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenothiazine | HCID 7108 | — |
| 反応物 | Triisopropyl phosphite | HCID 8304 | — |
| 反応物 | 3-Chloro-2-methyl-1-propene | HCID 11241 | — |
| 反応物 | Phosphite | HCID 107908 | — |
| 生成物 | Methallyl phosphonic acid diisopropyl ester | HCID 13953151 | — |
反応手順
208 parts of triisopropyl phosphite, 1.5 parts of phenothiazine and 3.4 parts of Ni(CO)4 (corresponding to 2 mol %, based on the phosphite) are heated to 120°-130° C in a nitrogen atmosphere. 99 parts (corresponding to a 10% excess) of methallyl chloride are added dropwise over a period of 5 hours. 68 parts of isopropyl chloride (Bp: 35°-36° C) are distilled off through a column. The product is fractionated in vacuo through a column. Boiling point: 58°-63° C/0.25 Torr; Yield: 155 parts (70.5% of the theoretical): nD20 : 1.4312 Purity according to GC: 97.3%
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-8a9b74cc0103416abf1784aa9c51e649 |
| 出典メモ | uspto-grants-1977_04 |