関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzene, 1-bromo-4-ethynyl- | HCID 136603 | — |
| 反応物 | 4-Chloro-2-diisopropylaminomethyleneamino-5-iodopyrimidine | HCID 73446451 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-(4-Bromophenylethynyl)-4-chloro-2-diisopropylaminomethyleneaminopyrimidine | HCID 73446456 | 78.1% |
反応手順
A mixture of 0.5 g of 1-bromo-4-ethynylbenzene, 5.0 mL of triethylamine, 0.031 mg of copper iodide, 0.94 g of 4-chloro-2-diisopropylaminomethyleneamino-5-iodopyrimidine and 0.046 g of dichlorobis(triphenyl)phosphine palladium II was magnetically stirred at room temperature for 18 hrs. The mixture was diluted with acetonitrile, filtered and the filtrate evaporated in vacuo. The evaporated filtrate was dissolved in dichloromethane and loaded on a column of silica gel equilibrated in the same solvent. Cuts were monitored by thin layer chromatography. After initial cuts of brown colored eluates, the product subsequently eluted as yellow fractions. Like cuts were pooled and evaporated to give 0.84 g of 5-(4-bromophenylethynyl)-4-chloro-2-diisopropylaminomethyleneaminopyrimidine as a thick amber syrup.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07205297B2 |
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| 出典データセット | uspto-grants-2007_04 |
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| ORD ID | ord-6ec0d97fa2584cd3b1674bb15858e107 |
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| 出典メモ | uspto-grants-2007_04 |
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