化工社化工社 化学情報印刷レポート · 研究参考用
Ethyl Acetate → 7-bromo-4-methyl-1H-indole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4-Bromo-3-nitrotoluene | HCID 79224 | — |
| 反応物 | HCID 178418507 | HCID 178418507 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 7-bromo-4-methyl-1H-indole | HCID 18752862 | 56.1% |
反応手順
To 300 ml of a solution of 65.0 g (301 mmol) of 2-bromo-5-methylnitrobenzene in tetrahydrofuran was added 1 liter of a 1.0 M solution of vinyl magnesium bromide (1 mol) in tetrahydrofuran at −60° C. in a nitrogen atmosphere under stirring during 1 hour. To the reaction mixed solution were added a saturated aqueous solution of ammonium chloride and ethyl acetate, and the resulting insoluble matters were filtered off. The resulting filtrate was dried over magnesium sulfate, concentrated, and then the resulting residue was purified by a silica gel column chromatography to give 35.5 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06638964B2 |
| 出典データセット | uspto-grants-2003_10 |
| ORD ID | ord-f790f8298cae4e4d959ecdc02468e318 |
| 出典メモ | uspto-grants-2003_10 |