Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 3-Methylcaprolactam
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Caprolactam | HCID 7768 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-Methylcaprolactam | HCID 581216 | — |
반응 단계
To a solution of azepan-2-one (0.5 g, 4.42 mmol, 1 equiv) in anhydrous THF (20 mL) under nitrogen, was added n-BuLi (4.4 mL, 2.5 M in n-hexane, 11.06 mmol) dropwise at 0° C. The reaction mixture was kept at 0° C. for 2 h, then MeI (0.3 mL, 4.86 mmol) was added. After stirring for 1 h, the mixture was quenched with water and extracted with DCM (2×50 mL). The combined organic layers were dried over anhydrous Na2SO4. After filtration and concentration, the crude product was directly used for the next step without further purification. MS (ESI): 128 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08772301B2 |
| 출처 데이터셋 | uspto-grants-2014_07 |
| ORD ID | ord-44149ac55fb24e058dd4632cdc8e51fd |
| 출처 메모 | uspto-grants-2014_07 |