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Formaldehyde → Ethyl 2-(4-bromophenyl)acrylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 2-(4-bromophenyl)acetate | HCID 7020609 | — |
| 触媒 | Tetrabutylammonium Chloride | HCID 70681 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 2-(4-bromophenyl)acrylate | HCID 11470828 | 73% |
反応手順
To a solution of (4-bromo-phenyl)-acetic acid ethyl ester (972.4 mg, 4 mmol), paraformaldehyde (240 mg, 8 mmol), and Bu4NCl (22 mg, 0.08 mmol) in DMF (10 mL) was added K2CO3 (1.32 g, 9.6 mmol). This mixture was heated at 60 degrees Celsius for 2 h. Then the mixture was cooled and diluted with EtOAc (30 mL) and washed with water (20 mL×3), brine, dried over Na2SO4, filtered and evaporated. The residue was purified by flash column chromatography on silica gel to give a white solid (0.74 g, 73%). MS: calc'd 255 (MH+), exp 255 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08202866B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-2924d033d258401fa7149898a5d9ffb3 |
| 出典メモ | uspto-grants-2012_06 |