Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl Ether → n-Ethyl-2-chloro-6-(1,1-dimethylethoxy)benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| 반응물 | Magnesium Bromide | HCID 82241 | — |
| 반응물 | 2-chloro-N-ethylbenzamide | HCID 347962 | — |
| 반응물 | t-Butylperoxy benzoate | HCID 21744378 | — |
| 반응물 | CID 53628100 | HCID 178418400 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | n-Ethyl-2-chloro-6-(1,1-dimethylethoxy)benzamide | HCID 18630260 | 33.2% |
반응 단계
To a solution of the compound of Example f (3.7 g, 20 mmol) and TMEDA (6.0 mL, 40 mmol) in anhydrous THF (100 mL) at -78° C. under nitrogen was added dropwise 1.3M s-BuLi (34 mL, 44 mmol). After 30 min MgBr2.Et2O (15.5 g, 60 mmol) was added, and the solution was warmed to ambient temperature, then cooled to -78° C. and stirred for 1 h. t-Butylperoxy benzoate (4.3 g, 22 mmol) was added, and the solution was warmed to -30° C. and worked up in the usual manner. Purification by HPLC with 3:17 ethyl acetate/hexanes gave 1.7 g of the desired compound as a white solid, a yield of 33%. m.p. 126-127° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06133252 |
| 출처 데이터셋 | uspto-grants-2000_10 |
| ORD ID | ord-f9a294bb80e04efd8c8f861f64633f16 |
| 출처 메모 | uspto-grants-2000_10 |