関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | [6-(2-Methyl-[1,3]dioxolan-2-yl)-pyridin-2-yl]-methanol | HCID 66928639 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methanesulfonic acid 6-(2-methyl-[1,3]dioxolan-2-yl)-pyridin-2-ylmethyl ester | HCID 86649482 | — |
反応手順
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of [6-(2-methyl-[1,3]dioxolan-2-yl)-pyridin-2-yl]-methanol (729 mg, 3.74 mmol) in dry CH2Cl2 (10.0 mL) was treated at 0° C. with Et3N (0.67 mL, 4.83 mmol) followed by DMAP (46 mg, 0.37 mmol) and Ms-Cl (0.37 mL, 4.72 mmol). After stirring at 0° C. for 1 h, the reaction mixture was quenched with water (10 mL), extracted with CH2Cl2 (10 mL) and the combined org. extracts were dried over Na2SO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (70:30 to 50:50 hept-EA) gave the title compound as a pale yellow oil. LC-MS-conditions 02: tR=0.79 min; [M+H]+=274.39.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536209B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-4758c3e68a7d43f888e55d711618913e |
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| 出典メモ | uspto-grants-2013_09 |
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