Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Nitrogen → 2-Bromo-1-(4-methyl-3-nitrophenyl)ethan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | 4-Methyl-3-nitrobenzoyl chloride | HCID 66323 | — |
| 반응물 | Trimethylsilyldiazomethane | HCID 167693 | — |
| 반응물 | Acetic Acid Mixture with Hydrobromic Acid | HCID 21893785 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Bromo-1-(4-methyl-3-nitrophenyl)ethan-1-one | HCID 3800422 | 93.8% |
반응 단계
To a stirred solution of 4-methyl-3-nitrobenzoyl chloride (Sigma-Aldrich, 2.0 g, 10 mmol) in CH2Cl2 (50 mL) is added trimethylsilyldiazomethane (2.0 M in hexanes, 40 mmol). The mixture is stirred for 2 hours at room temp, then cooled to 0° C. and a solution of HBr/HOAc (6.33 mL, 33% of HBr in HOAc, 35 mmol) is added dropwise (N2 evolution). After addition the mixture is stirred at 0° C. for 5 minutes, concentrated and purified by silica gel chromatography (CH2Cl2) to give the title compound (2.42 g, 93% yield) as a light yellow solid: Rf 0.61 (CH2Cl2)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08871767B2 |
| 출처 데이터셋 | uspto-grants-2014_10 |
| ORD ID | ord-d233ac288c324ac69bad3ac68f696d43 |
| 출처 메모 | uspto-grants-2014_10 |