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1-Chloroethyl chloroformate → 4-Propenylidenepiperidine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Chloroethyl chloroformate | HCID 521305 | — |
| 反応物 | 1-Benzyl-4-propylidenepiperidine | HCID 14966655 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 4-Propenylidenepiperidine hydrochloride | HCID 86752040 | 110.4% |
反応手順
There was dissolved 4.5 g (21 mmol) of 1-benzyl-4-propylidenepiperidine in 20 ml of dichloroethane and thereto 2.8 ml (25 mmol) of 1-chloroethyl chloroformate was added dropwise under cooling with ice. The reaction solution was stirred at room temperature for 30 minutes and then refluxed with heating for 30 minutes. The reaction solution was concentrated to 10 ml by removing the solvent under reduced pressure, and thereto was added 60 ml of methanol and the obtained mixture was refluxed with heating for 12 hours. The solvent was removed under reduced pressure to obtain 3.7 g of the titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05716969 |
| 出典データセット | uspto-grants-1998_02 |
| ORD ID | ord-c4cc18d6c77743f2bbfb66d9088d7a7c |
| 出典メモ | uspto-grants-1998_02 |