関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | 2,4-Dimethyl-3-pyridinemethanol | HCID 10329351 | — |
| 反応物 | HCID 178429541 | HCID 178429541 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178429437 | HCID 178429437 | 64% |
反応手順
(2,4-dimethylpyridin-3-yl)methanol was dissolved in dichloromethane (100 mL). Tribromophosphane (1.5 mL, 16 mmol) was added slowly. After 2 hours, the mixture was evaporated to dryness. The crude solid was dissolved in cold ethanol (100 mL), and 6-methyl-2-sulfanylpyrimidin-4-ol (1.13 g, 8.0 mmol) and triethylamine (4.5 mL, 32 mmol) were added. The resulting mixture was stirred at room temperature for 3 hours. The solvent was evaporated, and the crude solid was washed with THF (200 mL). After evaporation of solvent, the crude was purified by CombiFlash (0-6% MeOH in DCM) to provide 2-{[(2,4-dimethylpyridin-3-yl)methyl]sulfanyl}-6-methylpyrimidin-4-ol (2.5 g, 64% yield); 1H NMR (500 MHz, DMSO-d6): δ 2.23 (s, 3H), 2.68 (s, 3H), 2.84 (s, 3H), 4.62 (s, 2H), 6.05 (br, 1H), 7.71 (s, 1H), 8.62 (s, 1H); M+ 232.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09040538B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-24bd45339ce04bd4967a1437bf2ff7b0 |
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| 出典メモ | uspto-grants-2015_05 |
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