関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | 2-Hydroxy-4-[4-(3-hydroxy-prop-1-ynyl)-benzylamino]-benzoic acid methyl ester | HCID 58685831 | — |
| 溶媒 | Oxolane--water (1/1) | HCID 21881883 | — |
| 生成物 | 2-Hydroxy-4-[4-(3-hydroxy-prop-1-ynyl)-benzylamino]-benzoic acid | HCID 9971841 | 17.3% |
反応手順
2-Hydroxy-4-[4-(3-hydroxy-prop-1-ynyl)-benzylamino]-benzoic acid methyl ester (22 mg; 0.07 mmol) was dissolved in THF/H2O (1 mL/0.25 mL) and LiOH was added (17 mg; 0.7 mmol). The reaction mixture was heated to 90° C. for 1 hour. THF was removed by evaporation and EtOAc (3 mL) and H2O (0.5 mL) was added. The organic phase was isolated, dried (Na2SO4), filtered, evaporated to dryness and purified by flash column chromatography (SiO2-PE80-100° C./EtOAc/CH3COOH=1:1:1%) to yield 3.6 mg (17%) of pure product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07741352B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-f0f357f9ec75423a8a0a3472c5a90508 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|