関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Chloride | HCID 6327 | — |
| 反応物 | 2,4-Dimethoxybenzoyl chloride | HCID 2734719 | — |
| 反応物 | 6-methoxy-(6H)-dibenz[c,e][1,2]-oxaphosphorin | HCID 11436148 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 6-(2,4-Dimethoxybenzoyl)-(6H)-dibenz[c,e][1,2]-oxaphosphorin 6-oxide | HCID 14366288 | — |
反応手順
35.1 g (0.175 mol) of 2,4-dimethoxybenzoyl chloride were warmed to 70° C. under a nitrogen atmosphere. 40.3 g (0.175 mol) of 6-methoxy-(6H)-dibenz[c,e][1,2]oxaphosphorin were added dropwise in the course of two hours while stirring. The temperature was then slowly increased to 110° C. It was kept at this temperature until evolution of methyl chloride could no longer be detected. After cooling to 60° C., 70 ml of toluene were added. After crystallization, 50 g (75% of theory) of the abovementioned compound of melting point 112° to 115° C. were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05096935 |
|---|
| 出典データセット | uspto-grants-1992_03 |
|---|
| ORD ID | ord-a4abe4278b5547bf9a6693bb97c0f528 |
|---|
| 出典メモ | uspto-grants-1992_03 |
|---|
