참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Lithium Carbonate | HCID 11125 | — |
| 반응물 | 5-(1,1-Dimethylethyl) hydrogen 6-methyl-4,5-pyrimidinedicarboxylate | HCID 67182510 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-(1,1-Dimethylethyl) 4-methyl 6-methyl-4,5-pyrimidinedicarboxylate | HCID 67184336 | 79.1% |
반응 단계
To a solution of 9.12 g (38 mmol) of the material from Step B in 100 mL of N,N-dimethyl formamide (DMF) was added 3.1 mL (50 mmol) of iodomethane and 3.7 g (50 mmol) of lithium carbonate. The reaction mixture was heated at 60° C. for 3 hours. After cooling the reaction mixture was partitioned between dichloromethane and water. The organic layer was dried (sodium sulfate) and the solvent was removed with a rotary evaporator and then a vacuum pump. The residue was purified by MPLC with a gradient of 20-30% ethyl acetate in hexanes as eluant to afford 7.58 g of the title compound as an off-white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07560564B2 |
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| 출처 데이터셋 | uspto-grants-2009_07 |
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| ORD ID | ord-945412e5f1a24566adb2db44b9eadcf2 |
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| 출처 메모 | uspto-grants-2009_07 |
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