Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Anhydride → 1-(5-Bromo-3-methyl-1H-indazol-1-yl)ethan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Isoamyl Nitrite | HCID 8053 | — |
| 반응물 | 18-Crown-6 | HCID 28557 | — |
| 반응물 | Potassium Acetate | HCID 517044 | — |
| 반응물 | 4-Bromo-2-ethylaniline | HCID 2801283 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 1-(5-Bromo-3-methyl-1H-indazol-1-yl)ethan-1-one | HCID 59127382 | — |
반응 단계
Acetic anhydride (4.73 ml) was added to the mixture of 4-bromo-2-ethylaniline (5.0 g) and KOAc (2.94 g) in CHCl3 (70 ml) and stirred for 30 minutes at reflux. Then isoamyl nitrite (6.65 ml) and 18-crown-6-ether (660 mg) was added to the reaction mixture and stirred for 12 h. under reflux. The reaction mixture was diluted with CHCl3, washed with water, and dried over sodium sulfate. After filtration and concentration, the residue was purified by silica gel chromatography (hexane/EtOAc), and crystallized from mixed solvent of hexane and CHCl3 to give intended compound as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08524730B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-7b5dffd064424629bd0d34f8d159136b |
| 출처 메모 | uspto-grants-2013_09 |