Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Carbon tetrabromide → 1-benzyl-4-(bromomethyl)-3-nitro-1H-pyrazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Carbon tetrabromide | HCID 11205 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | (1-benzyl-3-nitro-1H-pyrazol-4-yl)methanol | HCID 67963013 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-benzyl-4-(bromomethyl)-3-nitro-1H-pyrazole | HCID 67963012 | — |
반응 단계
Carbon tetrabromide (3.67 g, 11.1 mmol) and triphenylphosphine (2.43 mL, 11.1 mmol) were added to a solution of C3 (1.29 g, 5.53 mmol) in dichloromethane (150 mL), and the reaction was allowed to stir at RT for 18 hours. After being washed with water, the reaction mixture was dried over magnesium sulfate, filtered, and concentrated under reduced pressure. Silica gel chromatography (Gradient: 0% to 100% EtOAc in heptane) afforded C4 as a solid. Yield: 951 mg, 3.21 mmol, 58%. LCMS m/z 297.9 (M+1). 1H NMR (400 MHz, CDCl3) δ 4.60 (d, J=0.6 Hz, 2H), 5.32 (s, 2H), 7.28-7.32 (m, 2H), 7.36-7.41 (m, 3H), 7.52 (br s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08933095B2 |
| 출처 데이터셋 | uspto-grants-2015_01 |
| ORD ID | ord-3b9d97be8a1c4beba2a87f3b50bcc943 |
| 출처 메모 | uspto-grants-2015_01 |