関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 反応物 | Methyl 4-hydroxy-3-iodo-5-nitrobenzoate | HCID 21086206 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Methyl 3-amino-4-hydroxy-5-iodobenzoate | HCID 21086158 | 92.2% |
反応手順
To a mixture of methyl 4-hydroxy-3-iodo-5-nitrobenzoate (2.99 g) in ethanol (40 mL) was added tin (II) chloride (10 g) portion wise. After stirring for 1 h at reflux, the mixture was cooled to 0° C. and quenched by saturated potassium carbonate (100 mL). The mixture was filtered through diatomaceous earth and the filtrate was extracted with ethyl acetate (4×100 mL). The combined organic extracts were dried (sodium sulfate), filtered, and concentrated under reduced pressure to give 2.5 g of the title compound: 1H NMR (300 MHz, DMSO-d6) δ 7.50, 7.24, 3.75.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07176242B2 |
|---|
| 出典データセット | uspto-grants-2007_02 |
|---|
| ORD ID | ord-851b94af2d2c479b9347162da1c190d6 |
|---|
| 出典メモ | uspto-grants-2007_02 |
|---|