関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | 2-Propen-1-ol, 3-(3,4-dichlorophenyl)- | HCID 53709191 | — |
| 触媒 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(3,4-Dichlorophenyl)-2-propene-1-ol acetate | HCID 53852844 | 97% |
反応手順
Treat a solution of the product of step 2 (13.2 g, 65 mmol) in CH2Cl2 (250 mL) at 0° C. with pyridine (7.89 mL, 97.5 mmol, 1.5 eq) and dimethylaminopyridine (397 mg, 3.25 0.05 eq), followed by CH3COCl (6.48 mL, 74.75 mmol, 1.15 eq). Allow the mixture to warm to 23° C., pour into 1M HCl (100 mL) and wash the resulting organic layer again with 1 M HCl (100 mL), followed by water (5×100 mL; pH=6.5-7). Dry the organic layer (Na2SO4) and concentrate to obtain 15.4 g (62.9 mmol, 97%) of 3-(3,4-dichlorophenyl)-2-propene-1-ol acetate as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05840725 |
|---|
| 出典データセット | uspto-grants-1998_11 |
|---|
| ORD ID | ord-596ba5ac38d843dda8fd994e96809546 |
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| 出典メモ | uspto-grants-1998_11 |
|---|
