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Ethyl bromoacetate → 4-(4-Methoxy-phenyl)-4-oxo-3-phenyl-butyric acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-(4-Methoxyphenyl)-2-phenylethan-1-one | HCID 231093 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-(4-Methoxy-phenyl)-4-oxo-3-phenyl-butyric acid ethyl ester | HCID 13441509 | 99% |
反応手順
A suspension of NaH (12.8 mmol, 512 mg) in DMSO (23 mL) was added 4′-methoxy-2-phenylacetophenone (12.8 mmol, 2.89 g) in 10 ml toluene dropwise under argon. After 30 minutes of stirring, ethyl bromoacetate (1.4 mL, 1 eq.) in 10 mL of toluene was added and the mixture was stirred at rt overnight. The reaction was quenched by addition of 2N HCl (4 mL), and then 60 mL of water. The mixture was extracted with CH2Cl2 (3×30 mL), dried over MgSO4 and concentrated under vacuum overnight to afforded 4.0 g (99%) of 4-(4-methoxy-phenyl)-4-oxo-3-phenyl-butyric acid ethyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08247414B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-1a501fcd1f934606885534729d3b3c5d |
| 出典メモ | uspto-grants-2012_08 |