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 | trans-2-(4-Bromobenzoyl)cyclopropanecarboxylic acid | HCID 58681322 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl trans-2-(4-bromobenzoyl)cyclopropanecarboxylate | HCID 58681311 | 83.5% |
反応手順
To a solution of trans-2-(4-bromobenzoyl)cyclopropanecarboxylic acid (9.43 g, 32.59 mmol) in MeOH (200 mL) was added 2,2-dimethoxypropane (10.18 g, 97.77 mmol) and HCl (4.0 M in dioxane, 4.0 mL). The resulting solution was stirred at 40° C. overnight, 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 trans-2-(4-bromobenzoyl)cyclopropanecarboxylate (7.7 g, 83%). 1H NMR (400 MHz, CD2Cl2) δ 1.68 (m, 2H), 2.37 (m, 1H), 3.21 (m, 1H), 3.65 (s, 3H), 7.68 (m, 2H), 7.90 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07091228B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-8a764fe4df3f4c62aea42b76e9d94364 |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|