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Pyridine → 2-(Trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 2-(Trimethylsilyl)ethanol | HCID 18013 | — |
| 反応物 | Benzoyl chloride, 3-(chlorosulfonyl)- | HCID 77671 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate | HCID 86676334 | — |
反応手順
To a mixture of 23.9 g of 3-(chlorosulfonyl)benzoyl chloride, 7.9 mL of pyridine, and 100 mL of dichloromethane was added dropwise 14 mL of 2-(trimethylsilyl)ethanol under ice-cooling, followed by stirring at room temperature for 2 hours. To the reaction mixture was added water, followed by extraction with chloroform, and the organic layer was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 29.4 g of 2-(trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09284295B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-fd932769b76a47e3ae3b4ecb47ed0316 |
| 出典メモ | uspto-grants-2016_03 |