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m-Chloroperbenzoic acid → 3-Methanesulfonyl-5-phenylethynylpyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | sodium thiosulfite anhydrous | HCID 15847209 | — |
| 反応物 | 3-Methylsulfanyl-5-phenylethynylpyridine | HCID 67047829 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Methanesulfonyl-5-phenylethynylpyridine | HCID 67047459 | 64% |
反応手順
Add 3-chlorobenzenecarboperoxoic acid (79.2 mg, 0.46 mmol) to a solution of 3-methylsulfanyl-5-phenylethynyl-pyridine, (prepared as described in EXAMPLE 128), (34.4 mg, 0.15 mmol) in dichloromethane (1 mL) at 0° C., warm to room temperature and stir for 2 h. Dilute with a 5% aqueous solution of sodium thiosulfite and dichloromethane. After separating the layers, sequentially wash the organic layer with a 5% aqueous solution of sodium thiosulfite and an aqueous saturated solution of sodium chloride, dry (magnesium sulfate), filter and concentrate. Purify the residue by silica gel chromatography, eluting with 100:0 to 100:50 hexanes:ethyl acetate, to give the title compound (24.8 mg, 64%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07915424B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-2aba3d60f40440ab85220b3af4fb4b61 |
| 出典メモ | uspto-grants-2011_03 |