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Dimethylformamide → Propan-2-yl 3-(2-fluorophenyl)prop-2-enoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | o-Fluorobenzaldehyde | HCID 67970 | — |
| 反応物 | (Ethoxycarbonylmethyl)triphenylphosphonium bromide | HCID 73731 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Propan-2-yl 3-(2-fluorophenyl)prop-2-enoate | HCID 57870847 | 60% |
反応手順
400 mg of sodium hydride (60% in oil, 10 mmol) were added to a stirred solution of 4.4 g of ethoxycarbonylmethyltriphenylphosphonium bromide (10 mmol) in 20 ml of DMF and the mixture was stirred further at RT for 10 min. 1.24 g of 2-fluoro-benzaldehyde (10 mmol) were added and the mixture was stirred for 5 h at RT. The reaction mixture was taken up in 100 ml of ethyl acetate and washed with a common salt solution, dried over sodium sulfate, filtered and concentrated under reduced pressure. Purification took place using a silica gel chromatography (ethyl acetate/heptane 1:1). 1.25 g of the title compound were obtained. Yield: 60%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08097758B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-964fca885af645dab3e1b47b2191ea3b |
| 出典メモ | uspto-grants-2012_01 |