Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 4-Cbz-1-methyl-2-piperazinone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Benzyl 3-oxopiperazine-1-carboxylate | HCID 736777 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-Cbz-1-methyl-2-piperazinone | HCID 58638540 | 66% |
반응 단계
To a solution of 3-oxo-piperazine-1-carboxylic acid benzyl ester (2.00 g, 8.54 mmol) in DMF (30 mL) was added KOtBu (1.54 g, 13.7 mmol) under Ar. The resulting solution was stirred at room temperature for 15 min and cooled to 0° C. MeI (0.85 mL, 14 mmol) was then added dropwise. The reaction mixture was allowed to warm to room temperature and stirred for 3 h. DMF was removed in vacuo and the residue was chromatographed on silica (5-50% EtOAc:hexane) to obtain the title compound (1.40 g, 66%). 1H-NMR (CDCl3; 400 MHz): δ 7.32 (m, 5H), 5.13 (s, 2H), 4.13 (s, 2H), 3.70 (m, 2H), 3.34 (m, 2H), 2.97 (s, 3H)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07705042B2 |
| 출처 데이터셋 | uspto-grants-2010_04 |
| ORD ID | ord-ebc6365f48494669a8f43f49246418fa |
| 출처 메모 | uspto-grants-2010_04 |