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Triethylamine → Methanesulfonic acid 2-phenyl-allyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | beta-Methylenephenethyl alcohol | HCID 80106 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methanesulfonic acid 2-phenyl-allyl ester | HCID 86653276 | 94.8% |
反応手順
To a well stirred solution of 2-phenyl-prop-2-en-1-ol (700 mg, 5.22 mmol) in dichlorometane (10 mL) at 0° C. is added triethylamine (0.945 mL, 6.78 mmol) and methylsulfonyl chloride (0.424 mL, 5.48 mmol). The reaction is allowed to stir for 10 min, warmed to room temperature and is stirred for 30 min. The reaction is quenched by the addition of a saturated aqueous solution of ammonium chloride and extracted several times with ethyl acetate. The organic layers are combined, washed with 1 N hydrochloric acid, brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The residue is purified via silica gel chromatography (10% ethyl acetate in hexanes) to yield the title compound (1.07 g, 4.95 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08841291B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-70d466be53c046c28b3842119842f724 |
| 出典メモ | uspto-grants-2014_09 |