化工社化工社 化学情報印刷レポート · 研究参考用
Trimethylamine → 4,4'-Bis(propargyloxycarbonyloxy)biphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylamine | HCID 1146 | — |
| 反応物 | 4,4'-Dihydroxybiphenyl | HCID 7112 | — |
| 反応物 | Propargyl chloroformate | HCID 3356829 | — |
| 反応物 | Water methylene chloride | HCID 21908982 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4,4'-Bis(propargyloxycarbonyloxy)biphenyl | HCID 19786007 | 93.6% |
反応手順
A flask equipped with a stirrer, thermometer, nitrogen gas tube and reflux condenser was charged with 18.6 g of 4,4'-dihydroxybiphenyl and 23.0 g of trimethylamine in 50.0 g of methylene chloride. To the flask was added 26.0 g of propargyl chloroformate dropwise over one hour and the mixture was allowed to react for 6 hours at 30° C. After the reaction, the reaction mixture was treated with methylene chloride-water mixture and the organic phase was separated followed by drying over magnesium sulfate overnight. After filtering, the filtrate was evaporated in a rotary evaporator. The resulting crystals were recrystallized to give the title compound at a yield of 93.6% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05258542 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-c984bd9a0c75459e93b03c8cf25efca2 |
| 出典メモ | uspto-grants-1993_11 |