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Tetrahydrofuran → (5-Chloropyridin-2-yl)methyl methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | (5-Chloropyridin-2-yl)methanol | HCID 20537893 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (5-Chloropyridin-2-yl)methyl methanesulfonate | HCID 70700476 | 99% |
反応手順
Triethylamine (12 mL) and methanesulfonyl chloride (5.7 mL) were added to tetrahydrofuran (150 mL) solution of 5-chloro-2-hydroxymethylpyridine (12.77 g) under cooling with ice, and stirred for 30 minutes under cooling with ice. After addition of water (150 mL), the reaction liquid was extracted with ethyl acetate (150 mL+150 mL), and the organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the residue was crystallized from ethyl acetate-diisopropyl ether mixed solvent to provide the title compound (14.65 g, 99%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732456B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-9a5fbfe159bf429d946f028309c04113 |
| 出典メモ | uspto-grants-2010_06 |