関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,2-Dimethoxypropane | HCID 6495 | — |
| 反応物 | cis-2-(4-Bromobenzoyl)cyclopropanecarboxylic acid | HCID 67147316 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl cis-2-(4-bromobenzoyl)cyclopropanecarboxylate | HCID 67147290 | 99.7% |
反応手順
To a solution of cis-2-(4-bromobenzoyl)cyclopropanecarboxylic acid (10.6 g, 36.63 mmol) in MeOH (250 mL) was added 2,2-dimethoxypropane (9.54 g, 91.59 mmol) and HCl (4.0 M in dioxane, 3.50 mL). The resulting solution was stirred at 40° C. for 3 days, and then evaporated to dryness. The resulting residue was purified by flash chromatography (Biotage Flash 40M) using 15 to 25% ethyl acetate in hexanes to afford methyl cis-2-(4-bromobenzoyl)-cyclopropanecarboxylate (10.34 g, 99%). 1H NMR (400 MHz, CD2Cl2) δ 1.39 (m, 1H), 1.82 (m, 1H), 2.34 (m, 1H), 2.77 (m, 1H), 3.54 (s, 3H), 7.65 (m, 2H), 7.89 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091228B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-2fd5618e389a417881c57b535e63dc15 |
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| 出典メモ | uspto-grants-2006_08 |
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