Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 1-(2,2-Dimethoxyethyl)-piperidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 5-Chlorovaleryl chloride | HCID 74089 | — |
| 반응물 | Aminoacetaldehyde dimethyl acetal | HCID 89728 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | Sodium Carbonate | HCID 10340 | — |
| 생성물 | 1-(2,2-Dimethoxyethyl)-piperidin-2-one | HCID 21978509 | 80.9% |
반응 단계
To a stirred mixture of aminoacetaldehyde dimethylacetal (0.74 g, 7 mmole) in ethyl acetate (20 mL) and 2M sodium carbonate (20 mL) was added 5-chlorovaleryl chloride (1.55 g, 10 mmole). The reaction mixture was stirred at ambient temperature for 1 hour. The aqueous layer was separated and extracted with ethyl acetate. The combined organic phase was washed with 1% hydrochloric acid and water, dried (magnesium sulfate), and concentrated. The oily residue was dissolved in tetrahydrofuran, and sodium hydride (60% in oil) (0.3 g, 7.5 mmole) was added. The reaction mixture was heated under reflux for 1.5 hours and filtered. The filtrate was concentrated to give 1-(2,2-dimethoxyethyl)-piperidin-2-one (1.06 g) as a pale yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07094778B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-1a741121a16944648d852fb3d307e1e8 |
| 출처 메모 | uspto-grants-2006_08 |