Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → Methyl 5-(2,2-difluoroethoxy)-2-nitrobenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,2-Difluoroethan-1-ol | HCID 136187 | — |
| 반응물 | 2,8,9-Triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo(3.3.3)undecane | HCID 4571243 | — |
| 반응물 | 5-Fluoro-2-nitrobenzoic acid methyl ester | HCID 5152049 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Methyl 5-(2,2-difluoroethoxy)-2-nitrobenzoate | HCID 59587324 | 92.5% |
반응 단계
8.53 g of 2,2-difluoroethanol are added to a solution of 17.31 g of methyl 5-fluoro-2-nitrobenzoate, 9.64 g of NEt3 and 32.71 g of 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane in 250 ml of anhydrous THF. The mixture is stirred at AT for 30 min. The solvent is evaporated under reduced pressure. Water is added and extraction is carried out with AcOEt. The extract is washed with a 1N aqueous HCl solution, with water and then with a saturated NaCl solution. It is dried over MgSO4 and filtered, and the solvent is evaporated under reduced pressure to give 21 g of the expected product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846654B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-6a6caacef79c480cb678629b6f435790 |
| 출처 메모 | uspto-grants-2014_09 |