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1-Chloroethyl chloroformate → 4-Benzylidenepiperidine 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-benzylidenepiperidine | HCID 21843364 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 4-Benzylidenepiperidine hydrochloride | HCID 18539010 | 42.7% |
反応手順
There was dissolved 24.6 g (96 mmol) of 1-benzyl-4-benzylidenepiperidine in 200 ml of dichloroethane and thereto 11.1 ml (102 mmol) of 1-chloroethyl chloroformate was added dropwise under cooling with ice. The reaction solution was refluxed with heating for 30 minutes and then stirred at room temperature for 1.5 hours. The reaction solution was concentrated to 80 ml by removing the solvent under reduced pressure, thereto was added 200 ml of methanol and the obtained mixture was refluxed with heating for 12 hours. The solvent was removed under reduced pressure and to the obtained residue was added 100 ml of isopropyl ether and the precipitate was separated by filtration to obtain 8.6 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-28b37068acdc4ae4a559829bf9f32b71 |
| 出典メモ | uspto-grants-1998_02 |