Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Thiochroman → 6-[3-(1-Acetylpiperidin-4-yl)-1-oxopropyl]-3,4-dihydro-2H-1-benzothiopyran
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Thiochroman | HCID 137415 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 반응물 | 3-(1-Acetyl-4-piperidinyl)propionyl chloride | HCID 10465951 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | 6-[3-(1-Acetylpiperidin-4-yl)-1-oxopropyl]-3,4-dihydro-2H-1-benzothiopyran | HCID 19108480 | 81.6% |
반응 단계
To a mixture of 3,4-dihydro-2H-1-benzothiopyran (1.5 g) and 3-(1-acetylpiperidin-4-yl)propionyl chloride (2.18 g) in 1,2-dichloroethane (20ml) was added aluminum chloride (3.2 g) portionwise at 10°-15° C. The mixture was stirred at room temperature for 2 hours then refluxed for additional 2 hours, and poured into icewater. The mixture was extracted with dichloromethane, washed with water, dried over anhydrous sodium sulfate. The solvent was distilled off. The residue was purified by silica gel column chromatography (developing solvent: ethyl acetate) to obtain 2.7 g of the title compound as a pale yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05273974 |
| 출처 데이터셋 | uspto-grants-1993_12 |
| ORD ID | ord-fcb979243cbd468aaea38beb0bf9cc98 |
| 출처 메모 | uspto-grants-1993_12 |