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3-Methylcatechol → 4-Methyl-1,3-benzodioxole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Methylcatechol | HCID 340 | — |
| 反応物 | Dibromomethane | HCID 3024 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Dibromomethane | HCID 3024 | — |
| 生成物 | 4-Methyl-1,3-benzodioxole | HCID 88560 | 111.7% |
反応手順
400 g of methylene bromide and 50 g of tetrabutylammonium bromide are taken under reflux in a stirred apparatus and a solution of 400 ml of water, 130 g of sodium hydroxide and 200 g of 3-methylpyrocatechol are added dropwise in the course of 5 hours. At the end of the addition, the mixture is subsequently stirred for a further 2 hours, cooled and extracted with methylene chloride. The organic phase is dried and distilled on a column. After first runnings of unreacted methylene bromide, 175 g of 4-methyl-1,3-benzodioxole are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04886816 |
| 出典データセット | uspto-grants-1989_12 |
| ORD ID | ord-39cf905349a1490b964adf50371d4526 |
| 出典メモ | uspto-grants-1989_12 |