Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cesium carbonate → 2-Chloro-5-(2,2-dimethylpropoxy)pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Propane, 1-iodo-2,2-dimethyl- | HCID 84953 | — |
| 반응물 | 2-Chloro-5-hydroxypyridine | HCID 819821 | — |
| 용매 | Diglyme | HCID 8150 | — |
| 생성물 | 2-Chloro-5-(2,2-dimethylpropoxy)pyridine | HCID 59280220 | — |
반응 단계
5.2 g (40.0 mmol) 6-chloropyridin-3-ol, 11.9 g (60.0 mmol) 1-iodo-2,2-dimethylpropane, 19.6 g (60.0 mmol) cesium carbonate and 120 ml diethylene glycol dimethyl ether are divided into five portions of equal size and are reacted in portions at 160° C. for 4 h in a single mode microwave (CEM Explorer). Thereafter, the five reaction mixtures obtained are combined, the solid is filtered off and rinsed with diethylene glycol dimethyl ether and the filtrate and wash solutions are combined. The majority of the solvent is removed and 300 ml water are added to the concentrated solution (approx. 50 ml). The mixture is stirred for 30 min and the solid obtained is filtered off, washed once with water and dried under a high vacuum.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08653111B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-9515b47fdaa94e3b925ae0dc67765780 |
| 출처 메모 | uspto-grants-2014_02 |