関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Bromobenzyl alcohol | HCID 85141 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Bromo-3-[(methoxymethoxy)methyl]benzene | HCID 11447578 | 83% |
反応手順
To a tetrahydrofuran (100 mL) solution of 3-bromobenzyl alcohol (10 g, 54 mmol) was added sodium hydride (2.3 g, 98 mmol, 60% in oil) at room temperature. Then, chloromethyl methyl ether (5.2 g, 64 mmol) was added to this suspension, which was stirred for 15 minutes at 60° C. This mixture was partitioned into ethyl acetate and water. The organic layer was separated and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=8:1) to obtain the title compound (10 g, 83%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841327B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-4203a6b99c9c41c7b61a2107c2ecb1da |
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| 出典メモ | uspto-grants-2014_09 |
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