関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 6-Bromo-3-pyridinemethanol | HCID 6421249 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (6-Bromopyridin-3-yl)methyl methanesulfonate | HCID 59281142 | — |
反応手順
(6-Bromopyridin-3-yl)methanol (2.45 g, 13.0 mmol) was dissolved in dichloromethane (20 mL), cooled to 0° C. and treated successively with N,N-diisopropylethylamine (2.73 mL, 15.6 mmol, 1.2 equiv) and methanesulfonyl chloride (1.17 mL, 15.0 mmol, 1.15 equiv). After stirring for 30 minutes, the mixture was treated with ammonium chloride (10 mL, aqueous saturated) and warmed to ambient temperature. The mixture was poured into water (100 mL) and extracted with ethyl acetate (2×100 mL). The combined organic extracts were dried with sodium sulfate, filtered and concentrated in vacuo, providing the titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08293744B2 |
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| 出典データセット | uspto-grants-2012_10 |
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| ORD ID | ord-cbba3324145b413fa0356d76683a33d6 |
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| 出典メモ | uspto-grants-2012_10 |
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