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Methanol → 3-Bromo-4-methoxyaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 2-Bromo-4-nitroanisole | HCID 78870 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Bromo-4-methoxyaniline | HCID 961083 | 92.6% |
反応手順
2-Bromo-1-methoxy-4-nitrobenzene (2.50 g, 10.8 mmol), SnCl2.2H2O (12.2 g, 53.9 mmol), and MeOH (30 mL) were combined and allowed to stir for 3 h at ambient temperature. To the mixture was added H2O (100 mL) and EtOAc (100 mL) resulting in the formation of a thick emulsion. To this was added sat. aq. NaHCO3 (30 mL). The layers were separated and the aqueous layer was extracted with EtOAc (3×30 mL). The organics were combined and dried over MgSO4 before being filtered. Concentration of the filtrate in vacuo gave 2.02 g of an off-white solid. This material was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524767B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-5827e8b7eb0b4d538c8fd85ae94865b5 |
| 出典メモ | uspto-grants-2013_09 |