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Dibromomethane → 1-[Ethoxy(isothiocyanato)phosphoryl]oxyethane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dibromomethane | HCID 3024 | — |
| 反応物 | Diethyl chlorophosphate | HCID 13139 | — |
| 反応物 | Ammonium thiocyanate | HCID 15666 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Potassium | HCID 5462222 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | 1-[Ethoxy(isothiocyanato)phosphoryl]oxyethane | HCID 556832 | — |
反応手順
To a stirred slurry of 1.0 to 1.1 molar equivalent of anhydrous sodium, potassium or ammonium thiocyanate in about 50 ml to 100 ml of a solvent such as benzene, toluene, xylene, ehtylene dichloride, chloroform, methylene chloride or methylene bromide, is added one molar equivalent of diethoxyphosphoryl chloride of formula (II) at a temperature range of 5° C to 30° C and, preferably, 15° C to 25° C and the reaction mixture stirred for a period of time from 4 to 4 hours to yield diethoxyphosphinyl isothiocyanate of formula (III). The reaction is slightly exothermic and such exotherm easily is controlled by either adjusting the rate of addition of said phosphoryl chloride or by using a cooling bath, or by a combination of the two.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04065466 |
| 出典データセット | uspto-grants-1977_12 |
| ORD ID | ord-42c5bcb7ae604546b28f0cd5d812d266 |
| 出典メモ | uspto-grants-1977_12 |