참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Benzyl Bromide | HCID 7498 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 5-Bromo-6-chloropyrimidine-2,4-diol | HCID 589834 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1,3-dibenzyl-5-bromo-6-chloropyrimidine-2,4(1H,3H)-dione | HCID 59834797 | 97.5% |
반응 단계
To a stirring solution of 5-bromo-6-chloropyrimidine-2,4(1H,3H)-dione (9.4 g, 41.7 mmol) in DMF (100 mL) at room temperature under argon was added K2CO3 (12.7 g, 91.8 mmol), followed by benzyl bromide (10.5 mL, 88.3 mmol). The reaction mixture was stirred at 75° C. for 1.5 h. After the reaction mixture was cooled to room temperature, water (100 mL) and EtOAc (150 mL) were added. The layers were separated. The organic layer was washed with water (50 mL×2), followed by saturated aqueous NaCl (50 mL), then dried (MgSO4) and concentrated at reduced pressure to obtain crude product. This crude product was passed through a bed of silica gel eluted with CH2Cl2 to obtain 16.5 g of the title compound as a white solid. HPLC/MS: retention time=3.818 min, [M+H]30 =405.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07452892B2 |
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| 출처 데이터셋 | uspto-grants-2008_11 |
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| ORD ID | ord-333c4ebb3d714d62b7e6062c48d45270 |
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| 출처 메모 | uspto-grants-2008_11 |
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