참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Phosphorus oxybromide | HCID 24613 | — |
| 반응물 | 6-Phenyl-2-pyridone | HCID 87889 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Bromo-6-phenylpyridine | HCID 568679 | 76% |
반응 단계
A mixture of 6-phenyl pyridone (3 g, 17.5 mmol; prepared according to Example 6) and phosphoryl bromide (7.2 g, 25.0 mmol) is heated to 100° C. for 5 h. The cooled mixture is poured into water (40 ml) and the pH is adjusted to 9 by addition of saturated aqueous sodium carbonate. Then the layers are separated and the aqueous layer is extracted with ethyl acetate (50 ml). The combined organic layers are dried with anhydrous magnesium sulphate and the solvent is evaporated in vacuo. The crude product is crystallized from aqueous ethanol. Subsequent purification by flash chromatography (silica gel, hexane/ethyl acetate 9/1 v/v) gives 2-bromo-6-phenyl pyridine (3.1 g, 76% of th.) as light brown crystals with mp 50° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06008161 |
|---|
| 출처 데이터셋 | uspto-grants-1999_12 |
|---|
| ORD ID | ord-35f85b64668d492f987465c0c41694d3 |
|---|
| 출처 메모 | uspto-grants-1999_12 |
|---|