참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Methyl 3-Hydroxybenzoate | HCID 88068 | — |
| 반응물 | 2-Bromo-4-chloropyridine | HCID 2762836 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3-(2-Bromo-pyridin-4-yloxy)-benzoic acid | HCID 58167936 | — |
반응 단계
A mixture of 2-bromo-4-chloro-pyridine (200 mg, 1.04 mmol), methyl-3-hydroxybenzoate (158 mg, 1.04 mmol), cesium carbonate (507 mg, 1.56 mmol) in 10 ml of anhydrous DMSO was heated at 66° C. for 5 hours. The mixture was diluted with ethyl acetate (100 ml), washed with brine (3×50 ml), dried over Na2SO4 and evaporated to give a colorless oil. The oil was dissolved in MeOH (8 ml), and 2M NaOH solution (4 ml, 8 mmol) was added. The mixture was heated at 60° C. for 20 minutes, poured into 50 ml of water, and acidified to pH=4. The precipitates were filtered, washed with water and dried in vacuo to give 3-(2-bromo-pyridin-4-yloxy)-benzoic acid as white solid. Yield: 170 mg, 56%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09328103B2 |
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| 출처 데이터셋 | uspto-grants-2016_05 |
|---|
| ORD ID | ord-f29c056ee6d54b999a20a8210d7db75c |
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| 출처 메모 | uspto-grants-2016_05 |
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