Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → 2,2,2-Trichloroethyl {6-[acetyl(methyl)amino]pyridin-3-yl}carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| 반응물 | N-(5-aminopyridin-2-yl)-N-methylacetamide | HCID 59301435 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,2,2-Trichloroethyl {6-[acetyl(methyl)amino]pyridin-3-yl}carbamate | HCID 86625492 | 52.4% |
반응 단계
To a solution of N-(5-aminopyridin-2-yl)-N-methylacetamide (1.00 g, 6.06 mmol) and pyridine (1.47 ml, 18.2 mmol) in tetrahydrofuran (20 ml) was added 2,2,2-trichloroethyl chloroformate (1.25 ml, 9.09 mmol) with ice-cooling, the mixture was stirred for 0.5 hour with ice-cooling, the reaction mixture was poured into ice-water and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of hexane and ethyl acetate to obtain the desired product (1.08 g, 52.4%) as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07851473B2 |
| 출처 데이터셋 | uspto-grants-2010_12 |
| ORD ID | ord-d5f1869f2f9c408995a5b1d87642dedb |
| 출처 메모 | uspto-grants-2010_12 |