Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl Oxalate → Ethyl 2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl Oxalate | HCID 7268 | — |
| 반응물 | Ethanone, 1-(2,4,6-trimethylphenyl)- | HCID 15461 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | Ethyl 2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate | HCID 14945000 | 66.7% |
반응 단계
To a solution of 2', 4', 6'-trimethylacetophenone (15 g, 92.6 mmol) and diethyl oxalate (20 g, 139 mmol) in 500 mL of anhydrous toluene was cautiously added 7.4 g of NaH (60% dispersion in mineral oil). The reaction mixture was slowly heated to reflux under N2. It was refluxed for about 20 minutes, then cooled, poured into ice-cold aqueous HCl solution, and extracted with ether. The extracts were washed with brine, dried over Na2SO4, filtered through a short silica gel pad and concentrated to give 16.2 g of a red oil which was used in the next reaction without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05723608 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-54fc6a8a376c4fd9a41d798a9116e90e |
| 출처 메모 | uspto-grants-1998_03 |