関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-tert-Butyloxirane | HCID 92174 | — |
| 反応物 | 2,4,6-Trichloropyrimidin-5-ol | HCID 86667332 | — |
| 生成物 | HCID 86711759 | HCID 86711759 | 52% |
反応手順
A mixture of 2,4,6-trichloro-pyrimidin-5-ol (400 mg, 2.01 mmol) and 2-tert-butyl oxirane (3 mL) was heated at 100° C. for 3 hours before being cooled and concentrated in vacuo. The resultant residue was triturated in hot methanol and the insoluble material removed. The filtrate was concentrated in vacuo and the resultant residue was purified by column chromatography (SiO2, 0-15% ethyl acetate in cyclohexane) to give 3,3-Dimethyl-1-(2,4,6-trichloro-pyrimidin-5-yloxy)-butan-2-ol as a white solid (275 mg, 52%). 1H NMR (400 MHz, CDCl3): δ 4.28 (1H, dd, J=9.38, 2.19 Hz), 4.00 (1H, t, J=9.19 Hz), 3.76-3.69 (1H, m), 2.53 (1H, d, J=3.48 Hz), 0.95 (9H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09346817B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-2d53566aaa9845d286990760446641f1 |
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| 出典メモ | uspto-grants-2016_05 |
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