化工社化工社 化学情報印刷レポート · 研究参考用
p-Toluenesulfonic acid → 1,6-Hexanediol monomethyl ether acrylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Acrylic Acid | HCID 6581 | — |
| 反応物 | Dimethyl Ether | HCID 8254 | — |
| 反応物 | 6-Methoxyhexan-1-ol | HCID 12651699 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1,6-Hexanediol monomethyl ether acrylate | HCID 14693048 | — |
反応手順
803.6 grams of the monomethyl ether described in Part (A) above were azeotropically esterified with 629.8 grams acrylic acid in 254.6 grams toluene in the presence of 24 grams p-toluenesulfonic acid and inhibitors until no more water was collected. Conditions were 95°-98° C., nitrogen sparge in vacuo. On completion, the product was washed and neutralized with sodium carbonate. 900 ppm p-methoxyphenol (MEHQ) was added and the solvent removed at 80° C. with maximum vacuum in the presence of an air sparge. Filter aid was added and the product filtered at 60° C. to give a clear, yellow liquid having a viscosity of 6.5 cps and a Gardener color of 3. Equipment used was a 2 liter flask, thermometer, Dean-Stark condenser and sparge tube.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05243085 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-a9a5f08948ef490a8633b44f5ca2f366 |
| 出典メモ | uspto-grants-1993_09 |