참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | 2-Bromo-1-fluoro-4-nitrobenzene | HCID 69699 | — |
| 반응물 | 2(1H)-Pyrimidinone, tetrahydro- | HCID 74615 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-(2-Bromo-4-nitrophenyl)tetrahydropyrimidin-2(1H)-one | HCID 59586715 | — |
반응 단계
910 mg (9.09 mmol) of tetrahydropyrimidinone in 39 ml of DMSO are admixed at RT with 1.53 g (13.6 mmol) of potassium tert-butoxide, and the mixture is stirred at room temperature for 30 min. 2.00 g (9.09 mmol) of 2-bromo-1-fluoro-4-nitrobenzene are added and the mixture is stirred at 60° C. After 18 h, it is cooled and added to 600 ml of water and 160 ml of saturated aqueous sodium chloride solution. It is extracted three times with 300 ml each time of ethyl acetate, and the combined organic phases are dried over sodium sulfate. After filtration, the solvents are removed under reduced pressure and the residue is purified by chromatography on silica gel (60:1 dichloromethane/ethanol). This affords 481 mg (17% of theory) of the desired compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08198267B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-9f39347d968c465b9431cc946213fff9 |
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| 출처 메모 | uspto-grants-2012_06 |
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