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 | Sodium hydride | HCID 24758 | — |
| 반응물 | Benzyl 3-oxopiperazine-1-carboxylate | HCID 736777 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-Cbz-1-methyl-2-piperazinone | HCID 58638540 | 82% |
반응 단계
Dissolve 4-benzyloxycarbonylpiperazin-2-one (2 g, 8.6 mmol) in THF (10 mL). Add sodium hydride (236 mg, 9.4 mmol, 60% dispersion in mineral oil) in one portion and stir at room temperature for 30 min. Add iodomethane (0.8 mL, 13 mmol) and stir at room temperature overnight. Concentrate, add ethyl acetate and wash with water. Separate organic layer, wash with saturated aqueous sodium chloride, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with ethyl acetate) to give the title compound as a yellow oil (1.7 g, 82%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07618978B2 |
| 출처 데이터셋 | uspto-grants-2009_11 |
| ORD ID | ord-a3975763d88b46c092902f66e2dd8321 |
| 출처 메모 | uspto-grants-2009_11 |