참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | tert-Butyl acrylate | HCID 15458 | — |
| 반응물 | 2-Bromo-4-chloro-1-(difluoromethyl)benzene | HCID 66744942 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 131736321 | HCID 131736321 | 22.1% |
반응 단계
To a solution of Intermediate 14A (0.88 g, 3.64 mmol) in DMF (10 mL) was added tert-butyl acrylate (1.401 g, 10.93 mmol), TEA (1.270 mL, 9.11 mmol) and Pd(OAc)2 (0.082 g, 0.364 mmol). The reaction was warmed to 90° C. After 5 h, the reaction was cooled to rt and then filtered to remove the solid. The filtrate was diluted with EtOAc, washed with 1M HCl, saturated NaHCO3, and brine. The organic phase was dried over MgSO4, filtered and concentrated. Purification by normal phase chromatography gave Intermediate 14B (232 mg, 22% yield) as a tan oil. MS (ESI) m/z: 233.1 (M-tBu)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09394276B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_07 |
|---|
| ORD ID | ord-3acab4bd2b3b46d9938ce3b25ad3edac |
|---|
| 출처 메모 | uspto-grants-2016_07 |
|---|
