関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-(1-Cyclohexylcyclopropyl)methanamine | HCID 57324434 | — |
| 反応物 | 6-chloro-N-(2-methylphenyl)pyrimidine-4-carboxamide | HCID 59447093 | — |
| 生成物 | 6-[cyclohexyl(cyclopropylmethyl)amino]-N-(2-methylphenyl)pyrimidine-4-carboxamide | HCID 59447089 | — |
反応手順
A solution of 6-chloro-N-(2-methylphenyl)pyrimidine-4-carboxamide (Intermediate 18; 3.00 g; 12.11 mmol) in EtOH (30 ml) was treated with DIEA (4.17 ml; 24.2 mmol) and cyclohexyl-cyclopropanemethyl-amine (Chembridge; 3.71 g; 24.2 mmol) and heated at 160° C. for 1 h. At the end of addition the reaction mixture was concentrated in vacuo, diluted with water and extracted with EtOAc. The combined organic layers were washed with NH4Cl, NaHCO3 and brine, dried on magnesium sulfate and evaporated in vacuo to afford the title compound as a brown solid, which was purified by precipitation from cyclohexane to afford the title compound as a beige solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09150519B2 |
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| 出典データセット | uspto-grants-2015_10 |
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| ORD ID | ord-86e7fc18656e40bdb59da635b15c5d4a |
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| 出典メモ | uspto-grants-2015_10 |
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