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Morpholine → 3-(Morpholine-4-sulfonyl)benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzoic acid, 3-(chlorosulfonyl)- | HCID 77641 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(Morpholine-4-sulfonyl)benzoic acid | HCID 257476 | 52.1% |
反応手順
3-(Chlorosulfonyl)benzoic acid (250 mg, 1.133 mmol) was added to morpholine (99 mg, 1.133 mmol) in the presence of potassium carbonate (313 mg, 2.266 mmol) in THF (5 mL) at room temperature, and reaction mixture allowed to stirred for 12 h at rt. The reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum, and then compound was purified by column chromatography (3% CH3OH/CH2Cl2) affording the title compound (160 mg) as a solid. 1H NMR (400 MHz, CD3OD): δ 8.34 (m, 1H), 8.32 (d, 1H, J=8.0 Hz), 7.99 (m, 1H), 7.76 (t, 1H, J=8.0 Hz), 3.70 (m, 4H), 2.98 (m, 4H). ESI-MS: 272.0 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08987335B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-ecaec209cb1f4c859c0307cebaa5c84c |
| 出典メモ | uspto-grants-2015_03 |