関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2,3-Dihydro-2,2-dimethyl-7-benzofuranol | HCID 15278 | — |
| 反応物 | 1-Chloroethyl chloroformate | HCID 521305 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Chloroethyl 2,3-dihydro-2,2-dimethyl-7-benzofuranyl carbonate | HCID 13557095 | 84% |
反応手順
21.5 g (0.15 mole) of 1-chloroethylchloroformate are added in a single portion to a solution of 2,3-dihydro-2,2-dimethyl-7-benzofuranol (24.6 g; 0.15 mole) in dichloromethane (150 ml). The mixture is cooled to between 0° and 5° C., and 12 g (0.15 mole) of pyridine are added dropwise. The mixture is stirred for 3 hours at 20° C. The organic phase is then washed with 2×50 ml of iced water. It is dried over magnesium sulphate and the solvent is evaporated. A yellow oil is obtained which is distilled. 34.1 g of the expected carbonate is then recovered (84% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04725680 |
|---|
| 出典データセット | uspto-grants-1988_02 |
|---|
| ORD ID | ord-3c480d95de8546edb218b0eba0488c82 |
|---|
| 出典メモ | uspto-grants-1988_02 |
|---|