関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 5-bromo-4-chloro-2-(2,5-dimethyl-1H-pyrrol-1-yl)-6-methylpyrimidine | HCID 59258848 | — |
| 反応物 | HCID 178479277 | HCID 178479277 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | HCID 178433070 | HCID 178433070 | 88% |
反応手順
A mixture of 5-bromo-4-chloro-2-(2,5-dimethyl-1H-pyrrol-1-yl)-6-methylpyrimidine (5.00 g, 17.0 mmol), cis-4-aminocyclohexanol hydrochloride (2.77 g, 18.3 mmol), and diisopropylethyl amine (8.69 mL, 49.9 mmol) in dimethylacetamide (60.0 mL) was heated at 160° C. in a sealed tube overnight. The reaction mixture was concentrated and the residue was purified by flash chromatography eluting with chloroform/methanol (0-3%). Combined fractions containing the desired product were concentrated. The resulting gum was dissolved in methyl tert-butyl ether (450 mL) and the solution was washed with 50% brine, dried (MgSO4), filtered and concentrated to afford the title compound as a orange foamy solid (5.53 g, 88%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07696213B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-a6395f4cfc864f66a4b39c5bca7257ce |
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| 出典メモ | uspto-grants-2010_04 |
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