참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 4,4,5,5-Tetramethyl-2-(4-nitrophenyl)-1,3,2-dioxaborolane | HCID 2773555 | — |
| 반응물 | Methyl 4-bromo-2-methylbenzoate | HCID 22031226 | — |
| 촉매 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl 3-methyl-4'-nitrobiphenyl-4-carboxylate | HCID 59385226 | — |
반응 단계
The compound of example 219 (10 g, 0.044 mol), 4,4,5,5-tetramethyl-2-(4-nitrophenyl)-1,3,2-dioxaborolane (13.16 gm, 0.0528 mole) and Pd(dppf)Cl2:CH2Cl2 (1.07 g, 0.00132 mol) were taken in DMF (250 mL) under an argon atmosphere. To this reaction mixture, degassed 2M solution of Na2CO3 (14 g, 0.132 mol, 66.5 mL) was added. The reaction mixture was stirred at 80-85° C. for 1 to 1.5 h. After completion of the reaction, water was added and the product obtained was extracted with ether. The combined ether layer was washed with brine and dried over anhydrous Na2SO4 or MgSO4. The solvent was evaporated and the product was purified by column (silica gel, 20% ethyl acetate in petroleum ether) to obtain the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08748426B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_06 |
|---|
| ORD ID | ord-f22d68aecef143089cc2c8ab56492826 |
|---|
| 출처 메모 | uspto-grants-2014_06 |
|---|
