関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Quinoline | HCID 7047 | — |
| 反応物 | 2,4,5-Trichlorophenol | HCID 7271 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Carbonochloridic acid, 2,4,5-trichlorophenyl ester | HCID 85650 | — |
反応手順
About 7 g of phosgene are passed into a solution of 10.0 g of 2,4,5-trichlorophenol in 50 ml of dichloromethane at 0° C., and the mixture is stirred at 0° C. for 15 min. 7.2 ml of quinoline in 20 ml of dichloromethane are added dropwise over the course of 30 min, and the orange-colored suspension is then stirred in an ice bath for 1 h. Subsequently nitrogen is passed through the suspension for 1 h in order to blow out excess phosgene (absorber tower). The mixture is subsequently filtered, and the filtrate is washed twice with water, dried, again filtered and evaporated to dryness in vacuo. The 4.45 g of oily brownish residue are relatively pure 2,4,5-trichlorophenyl chloroformate, which crystallizes in the refrigerator and can be employed without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05663141 |
|---|
| 出典データセット | uspto-grants-1997_09 |
|---|
| ORD ID | ord-dae3b58bc3fc481baebdcff7e34f3ebc |
|---|
| 出典メモ | uspto-grants-1997_09 |
|---|