Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Boron trifluoride etherate → Ethyl 3-methylidene-2-oxo-1-azacyclodecane-10-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Boron trifluoride etherate | HCID 8000 | — |
| 반응물 | Ethyl 3-(trimethylsilylmethyl)-3-hydroxy-2-oxo-1-azacyclodecane-10-carboxylate | HCID 19930812 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Ethyl 3-methylidene-2-oxo-1-azacyclodecane-10-carboxylate | HCID 19930803 | — |
반응 단계
Ethyl 3-(trimethylsilylmethyl)-3-hydroxy-2-oxo-1-azacyclodecane-10-carboxylate (0.98 g, 2.98 mmol) is dissolved in methylene chloride (50 mL), and boron trifluoride etherate (1.8 mL, 15 mmol) is added. The reaction is stirred at room temperature for 26 hours. The reaction is then quenched with saturated ammonium chloride and extracted several times with methylene chloride. The combined organic layers are dried (MgSO4), and the solvent is evaporated. The product is purified by silica gel chromatography (20% ethyl acetate/hexane) to give ethyl 3-methylidene-2-oxo-1-azacyclodecane-10-carboxylate, m.p. 91°-92° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05244889 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-33f9adfd6f284316b20090b99cc163ce |
| 출처 메모 | uspto-grants-1993_09 |