참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Acetic acid, 2-chloro-2,2-difluoro-, ethyl ester | HCID 67843 | — |
| 반응물 | 2-Bromo-5-nitrophenol | HCID 12867136 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Bromo-3-(difluoromethoxy)nitrobenzene | HCID 53415904 | — |
반응 단계
To a N2 purged round bottom flask was added 2-bromo-5-nitrophenol (29.0 g, 133 mmol, 1.0 eq.) followed by 16.8 mL (133 mmol, 1.0 eq) of ethyl chlorodifluoroacetate and 18.8 g of K2CO3 (133 mmol, 1.0 eq.). Anhydrous DMF (300 mL) was added and the mixture was stirred at 70° C. for 5 h. The mixture was cooled to RT and the solvent was removed. The obtained crude mixture was dissolved in CH2Cl2 (500 mL) and washed with 1 N NaOH (aq.). The organic layer was dried (MgSO4), filtered and evaporated. The crude material was further purified by column chromatography (0-5% EtOAc in hexanes) providing pure 1-bromo-2-difluoromethoxy-4-nitro-benzene.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07531553B2 |
|---|
| 출처 데이터셋 | uspto-grants-2009_05 |
|---|
| ORD ID | ord-a1dbb3c8f81b4fd0b726c1b5c355fe7c |
|---|
| 출처 메모 | uspto-grants-2009_05 |
|---|
