Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl acetopyruvate → HCID 59843200, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl acetopyruvate | HCID 88600 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 반응물 | Benzyl 4-(2-(1-bromo-2,2,2-trifluoroethylidene)hydrazinyl)piperidine-1-carboxylate | HCID 72576664 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 59843200 | HCID 59843200 | 38.6% |
반응 단계
To a stirred solution of Methyl 2,4-dioxopentanoate (892 mg, 6.19 mmol) in MeOH (11.5 mL) at room temperature was added Sodium methoxide (25% in MeOH, 0.891 mL, 4.13 mmol). Then a solution of 111 (842 mg, 2.063 mmol) in MeOH (2.3 mL) was added drop-wise and the suspension was stirred for 10 min at room temperature, then for 2 h at 65° C. After cooling, the mixture was taken to dryness and AcOEt and saturated NaHCO3 were added, the organic layer was separated, dried over MgSO4, filtrated and evaporated and the residue was purified via Biotage (10% to 40% EtOAc/Hexane; 25S column) to afford 112 (361 mg, 38.6% yield) as red oil. LRMS (ESI): calc. 453.4; found 454.2 (MH)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08338437B2 |
| 출처 데이터셋 | uspto-grants-2012_12 |
| ORD ID | ord-77022f1346174c788530c12e9d0ac4d5 |
| 출처 메모 | uspto-grants-2012_12 |