化工社化工社 化学情報印刷レポート · 研究参考用
Ammonium Hydroxide → 1,3-dimethyl-1H-pyrazole-4-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 1,3-dimethyl-1H-pyrazole-4-sulfonyl chloride | HCID 4635707 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,3-dimethyl-1H-pyrazole-4-sulfonamide | HCID 13342783 | 111.6% |
反応手順
A solution of 1,3-dimethyl-1H-pyrazole-4-sulfonyl chloride (232 mg, 1.192 mmol) in THF (10.0 mL) was cooled to 0° C. and to it was added dropwise ammonium hydroxide (0.650 mL, 16.69 mmol). The reaction mixture was allowed to warm to RT and left to stir over the weekend (ca. 64 hours). The reaction mixture was concentrated in vacuo. The residues were taken up in water, then neutralized with 1M aqueous HCl (dropwise addition) to pH 5-6 and extracted with ethyl acetate (3×50 mL). The combined organics were dried over MgSO4, filtered and evaporated to dryness, producing the title compound (233 mg). LCMS (A): m/z (M+H)+ 176, C5H9N3O2S requires 175 (acidic).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08877742B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-6d52788399694fb69f0a848ce112f179 |
| 出典メモ | uspto-grants-2014_11 |