関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Butyn-1-ol | HCID 12991 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4,5,6-Trichloropyrimidine | HCID 249007 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4,5-Dichloro-6-(2-butynyloxy)pyrimidine | HCID 22599751 | 90% |
反応手順
0.56 g of sodium hydride (60% oil suspension) was suspended in 18 ml of tetrahydrofuran. 2 ml of tetrahydrofuran solution of 0.8 g of 2-butyn-1-ol was added dropwise at room temperature therein slowly, and the mixture was stirred for 20 minutes. Into the mixture was added dropwise 5 ml of tetrahydrofuran solution of 3 g of 4,5,6-trichloropyrimidine at 0° C. slowly, and stirred for 2 hours. The reaction mixture was poured into a saturated ammonium chloride aqueous solution, and the mixture was extracted with ethyl acetate three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 2.23 g of 4,5-dichloro-6-(2-butynyloxy)pyrimidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732448B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-43ea41315637414b82cbceb2701829f2 |
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| 出典メモ | uspto-grants-2010_06 |
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