Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl malonate → 1,3-Dimethyl 2-(4-bromo-2-nitrophenyl)propanedioate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl malonate | HCID 7943 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Bromo-1-fluoro-2-nitrobenzene | HCID 2736328 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 1,3-Dimethyl 2-(4-bromo-2-nitrophenyl)propanedioate | HCID 15740596 | — |
반응 단계
To a solution of dimethyl malonate (7.8 mL, 68.2 mmol) in DME (100 mL) at 0° C. was added K2CO3 (12.6 g, 91.0 mmol). The reaction mixture was stirred for 30 min, and then 4-bromo-1-fluoro-2-nitrobenzene (10.0 g, 45.5 mmol) was added. The reaction mixture stirred at 40° C. overnight. The reaction was cooled, diluted with water (200 mL), and extracted with EtOAc (100 mL×3). The combined organic layers were washed with brine (100 mL), dried (Na2SO4) and concentrated. The residue was triturated with PE:EtOAc=8:1 (30 mL) to 13.0 g (86%) of the title compound as a yellow solid. [M+H] Calc'd for C11H10BrNO6, 332, 334. Found, 332, 334.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09447046B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-fd035b322cdf4f62b5b9261220c761a8 |
| 출처 메모 | uspto-grants-2016_09 |