関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Lithium Carbonate | HCID 11125 | — |
| 反応物 | 5-(1,1-Dimethylethyl) hydrogen 6-methyl-4,5-pyrimidinedicarboxylate | HCID 67182510 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-(1,1-Dimethylethyl) 4-methyl 6-methyl-4,5-pyrimidinedicarboxylate | HCID 67184336 | 79.1% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560564B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-945412e5f1a24566adb2db44b9eadcf2 |
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| 出典メモ | uspto-grants-2009_07 |
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