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Sodium Hydroxide → 1-Bromo-4-hydroxy-isoquinoline-3-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-Bromo-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester | HCID 86014541 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-Bromo-4-hydroxy-isoquinoline-3-carboxylic acid | HCID 86014613 | — |
反応手順
A mixture of 1-bromo-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester (8.18 g, 25 mmol; Example D-28 a) aqueous 2N NaOH (80 ml, 160 mmol) and EtOH (80 ml) was refluxed with stirring for 2 h. Then the solution was concentrated in vacuo to ½ of its volume, diluted with water (200 ml), and was acidified by addition of concentrated aqueous HCl. After stirring at ambient temperature for 1 h the resulting suspension was submitted to vacuum filtration. The filter cake was washed thoroughly with water and dried in vacuo at 75° C. to give the title compound as a white solid (6.10 g); 1H NMR (DMSO-d6): δ=8.30 to 8.37 (m, 1H), 8.16 to 8.22 (m, 1H), 7.93 to 8.03 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07323475B2 |
| 出典データセット | uspto-grants-2008_01 |
| ORD ID | ord-8d57052fe5134dce865adc831dc16613 |
| 出典メモ | uspto-grants-2008_01 |