Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → 1,1-Dimethylethyl N-[4-(bromomethyl)-2-pyridinyl]carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Carbon tetrabromide | HCID 11205 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 2-(Boc-amino)-4-(hydroxymethyl)pyridine | HCID 23151001 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1,1-Dimethylethyl N-[4-(bromomethyl)-2-pyridinyl]carbamate | HCID 22097736 | 62% |
반응 단계
Triphenylphosphine (970 mg, 3.7 mmol) and carbon tetrabromide (1.5 g, 4.6 mmol) were added to a solution of (2-tert-butoxycarbonylaminopyridin-4-yl)methanol (Reference compound No. 4-1, 690 mg, 3.1 mmol) in methylene chloride (20 mL) under ice-cooling, and the mixture was stirred for 2 hours at room temperature. Ethyl acetate (30 mL) was added to the reaction mixture, the whole was washed with saturated aqueous sodium hydrogen carbonate solution (20 mL) and brine (20 mL), and then dried over anhydrous magnesium sulfate. The organic layer was evaporated under reduced pressure, and the resulting solid was filtered off with ethyl acetate to give 550 mg of the title reference compound as a colorless solid. (Yield 62%)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07544703B2 |
| 출처 데이터셋 | uspto-grants-2009_06 |
| ORD ID | ord-0f5a3073906945fdb8b62484d3049fa9 |
| 출처 메모 | uspto-grants-2009_06 |