関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Allyl Alcohol | HCID 7858 | — |
| 反応物 | 1-Chloro-2-iodobenzene | HCID 11993 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 触媒 | Tetrabutylammonium Chloride | HCID 70681 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chlorocinnamaldehyde | HCID 3014042 | 74% |
反応手順
A mixture of 2.2 mL (18 mmol) of 2-chloroiodobenzene, 1.8 mL (27 mmol) of allyl alcohol, 81 mg (0.36 mmol) of Pd(OAc)2, 5.3 g (18 mmol) of Bu4NCl, and 3.8 g (45 mmol) of NaHCO3 in 50 mL of DMF is stirred under Ar2 at 30° C. for 24 h. Water is added and the mixture is extracted with EtOAc. The extract is washed with brine, dried over MgSO4, filtered and concentrated. Flash chromatography (0-50% EtOAc in hexanes) provides 2.2 g (74%) of 3-(2-chlorophenyl)propenal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08859814B2 |
|---|
| 出典データセット | uspto-grants-2014_10 |
|---|
| ORD ID | ord-6790add3008d4712b95d944557dca659 |
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| 出典メモ | uspto-grants-2014_10 |
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