Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → Ethyl 2-(4-acetoxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-3-oxo-butyrate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Acetyl chloride | HCID 6367 | — |
| 반응물 | Ethyl 3-(4-hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate | HCID 21982235 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Ethyl 2-(4-acetoxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-3-oxo-butyrate | HCID 21982267 | 54.2% |
반응 단계
Ethyl 3-(4-hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (102.4 mg, 0.34 mmol) was dissolved in dichloromethane, and pyridine (55 μl, 0.682 mmol) and acetyl chloride (49 μl, 0.68 mmol) were then slowly added dropwise to the obtained solution at 0° C. The resulting mixture was then stirred at the same temperature for 10 minutes. After the reaction was completed, the reaction mixture was washed with water and then the aqueous layer was extracted with dichloromethane. The combined organic layer was dried with anhydrous sulfate and distilled under a reduced pressure. The desired product (64 mg, 54%) was obtained by performing column chromatography (eluent: n-hexane/ethyl acetate=3/1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07094908B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-8ab64c3ee79f4ec68259b9f3e101f5c1 |
| 출처 메모 | uspto-grants-2006_08 |