関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | Benzoic acid, 3,5-dimethyl-, methyl ester | HCID 32786 | — |
| 触媒 | Titanium tetraphenoxide phenol | HCID 86752029 | — |
| 生成物 | Benzoic acid, 3,5-dimethyl-, methyl ester | HCID 32786 | — |
| 生成物 | Phenyl 3,5-dimethylbenzoate | HCID 19704462 | — |
反応手順
Into this autoclave were charged methyl 3,5-dimethylbenzoate 90 g (550 mmole), phenol 207 g (2200 mmole) and titanium tetraphenoxide/phenol adduct 2.8 g (5.5 mmole) in a state such that the phenol was melting. The autoclave was sealed and then cooled with ice. After sufficient cooling, the inner gas was evacuated with a vacuum pump. Then, the contents were heated and reacted for three hours at 230° C. Furthermore, during the reaction, the liquid held in the reservoir was continuously removed with a pump at a rate of 10 g per hour. After cooling, the reaction mixture in the autoclave was separated by distillation to obtain phenyl 3,5-dimethylbenzoate (product) in an amount of 85 g (68% yield in terms of methyl 3,5-dimethylbenzoate). The boiling point was 155° C./2 mmHg, and the melting point was 32° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05714627 |
|---|
| 出典データセット | uspto-grants-1998_02 |
|---|
| ORD ID | ord-e6cbd8c2ee7a4e58a36f8c4288f0b247 |
|---|
| 出典メモ | uspto-grants-1998_02 |
|---|