Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → Benzoic acid, acetylmethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Benzoyl chloride | HCID 7412 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Hydroxyacetone | HCID 8299 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Benzoic acid, acetylmethyl ester | HCID 23137 | 87.8% |
반응 단계
To a pyridine (25 ml) and THF (10 ml) solution of hydroxyacetone (5 g, 67.5 mmol), benzoyl chloride (12 ml, 103 mmol) was added dropwise at 0° C. in a nitrogen atmosphere and the mixture was stirred for 43 hours at room temperature. Ice was added to the reaction mixture, which was then diluted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, water, and a saline solution, dried over anhydrous sodium sulfate, and concentrated. The obtained crude product was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate=1/0-1/1 gradient). Desired fractions were concentrated to obtain the title compound (10.56 g, 87.8% yield) as a light yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07425634B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-dd0a4ec0dabe404984930a4985ccb38e |
| 출처 메모 | uspto-grants-2008_09 |