참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl chlorodifluoroacetate | HCID 73935 | — |
| 반응물 | Potassium Bromide | HCID 253877 | — |
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 반응물 | 1-Bromo-5-(tert-butyl)-4-methoxy-2-nitrobenzene | HCID 57470245 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-Tert-butyl-2-methoxy-5-(trifluoromethyl)-4-nitrobenzene | HCID 57470246 | 61.6% |
반응 단계
A mixture of 1-tert-butyl-2-methoxy-5-bromo-4-nitrobenzene (867 mg, 3.0 mmol), KF (348 mg, 6 mmol), KBr (714 mg, 6 mmol), CuI (684 mg, 3.6 mmol), methyl chlorodifluoroacetate (2.2 mL, 21.0 mmol) in DMF (5 mL) was stirred at 125° C. in a sealed tube overnight, cooled to room temperature, diluted with water and extracted three times with EtOAc. The combined organic layers were washed with brine and dried over anhydrous MgSO4. After removal of the solvent, the residue was purified by column chromatography (0-5% EtOAc-Hexane) to yield 1-tert-butyl-2-methoxy-5-(trifluoromethyl)-4-nitrobenzene (512 mg, 61%). 1H NMR (400 MHz, CDCl3) δ 7.60 (s, 1H), 7.29 (s, 1H), 3.90 (s, 3H), 1.33 (s, 9H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08829204B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-e77fe0383fc346d59ce7a71dd0be2d9e |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
