Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Carbon Tetrachloride → (4-Isopropyl-piperazin-1-yl)-(5-piperidin-1-ylmethylpyrazin-2-yl)-methanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Carbon Tetrachloride | HCID 5943 | — |
| 반응물 | Benzoyl Peroxide | HCID 7187 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | 2-Pyrazinecarboxylic acid, 5-methyl-, methyl ester | HCID 465065 | — |
| 반응물 | Methyl 5-(dibromomethyl)pyrazine-2-carboxylate | HCID 67188344 | — |
| 생성물 | (4-Isopropyl-piperazin-1-yl)-(5-piperidin-1-ylmethylpyrazin-2-yl)-methanone | HCID 11544498 | 31% |
반응 단계
5-Dibromomethyl-pyrazine-2-carboxylic acid methyl ester. 5-Methyl-pyrazine-2-carboxylic acid methyl ester (1.60 g, 10.5 mmol; Macdonald, S. J. F. et al. J. Med. Chem. 2002, 45(18):3878-3890.), N-bromosuccinimide (5.62 g, 31.6 mmol), and dibenzoyl peroxide (0.255 g, 1.05 mmol) were dissolved in CCl4 (80 mL). The mixture was heated at reflux for 18 h. The reaction mixture was cooled and washed with 10% aq. Na2SO3 (2×20 mL) and H2O (1×30 mL). The organic phase was dried over Na2SO4, filtered, and concentrated to yield a brown oily crude material (2.41 g). The crude product was purified (SiO2: 0-20% ethyl acetate/hexanes) to give the title compound (1.00 g, 31%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07947718B2 |
| 출처 데이터셋 | uspto-grants-2011_05 |
| ORD ID | ord-1e6cc00fb549435db6fa74da074c38f6 |
| 출처 메모 | uspto-grants-2011_05 |