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Cesium carbonate → 2-Chloro-5-(2,2-dimethylpropoxy)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Propane, 1-iodo-2,2-dimethyl- | HCID 84953 | — |
| 反応物 | 2-Chloro-5-hydroxypyridine | HCID 819821 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | 2-Chloro-5-(2,2-dimethylpropoxy)pyridine | HCID 59280220 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653111B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-9515b47fdaa94e3b925ae0dc67765780 |
| 出典メモ | uspto-grants-2014_02 |