関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromo-4-fluorobenzaldehyde | HCID 173604 | — |
| 反応物 | N-(4-chlorophenethyl)-4-hydroxybenzamide | HCID 60628097 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(4-chlorophenethyl)-4-(2-bromo-4-formylphenoxy)benzamide | HCID 86643286 | 71.2% |
反応手順
N-(4-chlorophenethyl)-4-hydroxybenzamide (1.5 g, 5.4 mmol) was diluted with DMSO (15 mL) followed by the addition of K2CO3 (0.89 g, 6.4 mmol) and 3-bromo-4-fluorobenzaldehyde (1.0 g, 4.9 mmol). The reaction was stirred at 85° C. overnight and then cooled to ambient temperature. The reaction mixture was diluted with ethyl acetate and washed with twice with 10% sodium carbonate, water and brine, and then concentrated. The crude material was purified by silica gel chromatography eluting with hexanes:ethyl acetate (1:1) and then 100% ethyl acetate to yield N-(4-chlorophenethyl)-4-(2-bromo-4-formylphenoxy)benzamide (1.6 g, 71% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08183289B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-1e7baa39cdbb4a42af63da61f22773e1 |
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| 出典メモ | uspto-grants-2012_05 |
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