化工社化工社 化学情報印刷レポート · 研究参考用
Dibenzothiophene → 2-Methyl-1,2-dihydrobenzo[b]indeno[4,5-d]thiophen-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dibenzothiophene | HCID 3023 | — |
| 反応物 | Methacryloyl chloride | HCID 13528 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Methyl-1,2-dihydrobenzo[b]indeno[4,5-d]thiophen-3-one | HCID 58795476 | — |
反応手順
20 g (108.7 mmol) of dibenzothiophene (1) were added at −78° C. to an agitated solution of 10.6 ml methacryloyl chloride (108.7 mmol) and 15.3 g AlCl3 (114.8 mmol) in 250 ml methylene chloride and brought to room temperature overnight. The solution was hydrolysed carefully at 0° C., the organic phase was separated, washed with an aqueous solution of K2CO3 and dried over Na2SO4. After removal of the solvent and crystallisation in toluene/pentane≈10:1, 2-methyl-1,2-dihydrobenzo[b]indeno[4,5-d]thiophen-3-one (2) was obtained as crystalline solid material (21.6 g, 85.9 mmol, 79%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07381679B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-a345638143464cd78cfc80c19d360cf3 |
| 出典メモ | uspto-grants-2008_06 |