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, 1.1 5 eq). Allow the mixture to warm to 23° C., pour into 1M HCl (100 mL) and wash the resulting organic layer again with 1M 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 | US05696267 |
|---|
| 出典データセット | uspto-grants-1997_12 |
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| ORD ID | ord-b33904e53c3e41ca94c5b75b0a6b519d |
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| 出典メモ | uspto-grants-1997_12 |
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