Methanol → 1-methanesulfonylmethyl-3-nitro-1H-pyrazole
反応式
O[O:2][S:3]([O-:5])=O.[K+].CS[CH2:9][N:10]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[N:11]1.[CH3:18]O>O>[CH3:18][S:3]([CH2:9][N:10]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[N:11]1)(=[O:5])=[O:2]参加物
5
実験手順
Oxone (2.05 g, 3.36 mmol) was added to a mixture of 1-methylsulfanylmethyl-3-nitro-1H-pyrazole (194 mg, 1.12 mmol) in methanol (10 mL) and deionized water (100 μL) was allowed to proceed for 16 h with vigorous stirring. The solvent was removed in vacuo and the crude material was purified by ISCO flash column chromatography (Teledyne Isco RediSep Flash Column 10 g; 0% ethyl acetate/hexanes to 50% ethyl acetate/hexanes) afforded 1-methanesulfonylmethyl-3-nitro-1H-pyrazole as a white solid (184 mg, 80%).
後処理
- customThe solvent was removed in vacuo
- customthe crude material was purified by ISCO flash column chromatography (Teledyne Isco RediSep Flash Column 10 g; 0% ethyl acetate/hexanes to 50% ethyl acetate/hexanes)
出典と根拠
- ORDレコード
- ord-56903b4f1b0e46bcb31c03c0654946db
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07935699B2
反応ノート
読み込み中…