関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 5-Chloro-salicylaldehyde | HCID 12481 | — |
| 反応物 | tert-Butyl 2-bromo-2-methylpropionate | HCID 90290 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(4-Chloro-2-formyl-phenoxy)-2-methyl-propionic acid tert-butyl ester | HCID 57566221 | 54.4% |
反応手順
To a solution of 5-chlorosalicylaldehyde (5 g, 32 mmol) in N,N-dimethylformamide (100 mL) was added 2-bromo-2-methyl-propionic acid tert-butyl ester (10.7 g, 48 mmol), Cs2CO3 (3.1 g, 95 mmol). The reaction mixture was heated at 140° C. for 18 h. The mixture was partitioned between ethyl acetate and water. The organic layer was separated, and aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with water, brine, dried over Na2SO4 and concentrated to give 2-(4-chloro-2-formyl-phenoxy)-2-methyl-propionic acid tert-butyl ester as a pale yellow solid (Yield 5.2 g, 54%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08217051B2 |
|---|
| 出典データセット | uspto-grants-2012_07 |
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| ORD ID | ord-0055460bcd0648c187ffb07034b7625b |
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| 出典メモ | uspto-grants-2012_07 |
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