Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Chloroethyl chloroformate → 4-Benzylidenepiperidine hydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Chloroethyl chloroformate | HCID 521305 | — |
| 반응물 | 1-Benzyl-4-benzylidenepiperidine | HCID 21843364 | — |
| 용매 | 1,1-Dichloroethane | HCID 6365 | — |
| 생성물 | 4-Benzylidenepiperidine hydrochloride | HCID 18539010 | 42.7% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05716969 |
| 출처 데이터셋 | uspto-grants-1998_02 |
| ORD ID | ord-28b37068acdc4ae4a559829bf9f32b71 |
| 출처 메모 | uspto-grants-1998_02 |