Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Oxalyl chloride → 2-Benzoyl-6-methylpyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 6-Methylpyridine-2-carboxylic acid | HCID 70282 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | Benzene | HCID 241 | — |
| 생성물 | 2-Benzoyl-6-methylpyridine | HCID 12623268 | — |
반응 단계
To 15 g of 6 -methyl-2-pyridylcarboxylic acid (122 mmol) in 200 ml benzene is added dropwise 19.1 g (150 mmol) oxalyl chloride (dissolved in 30 ml benzene) with ice bath cooling. After 1 hr, solvent and excess chloride are removed. Concentrate is taken up in 100 ml benzene, cooled to ~10° & 175 mmol AlCl3 added. The solution is heated to 25° for 1 hour, then heated to reflux for 2 hours, and finally cooled and stirred overnight. The mixture is poured onto ice/conc. HCl, then washed with ether. Fifty Percent (50%) sodium hydroxide is added until the precipitate is dissolved. The solution is extracted with CHCl3, washed with water, dried and stripped, leaving 6-benzoyl-2-methylpyridine.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04224330 |
| 출처 데이터셋 | uspto-grants-1980_09 |
| ORD ID | ord-0de59541749840e78a9cd561f168b847 |
| 출처 메모 | uspto-grants-1980_09 |