関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 6-(Chloromethyl)-2,4(1H,3H)-pyrimidinedione | HCID 73273 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 117824059 | HCID 117824059 | — |
反応手順
A mixture of 6-(chloromethyl)pyrimidine-2,4(1H,3H)-dione (1 g, 6.23 mmol), 2,2,2-trifluoroethanol (2.235 mL, 31.14 mmol) and cesium carbonate (6.09 g, 18.68 mmol) in dimethylformamide (10 mL) was heated in a microwave oven at 100° C. for 30 min. The mixture was filtered and the volatiles were removed in vacuum. The residue was treated with diluted HCl (pH 4.5) and cooled to 0° C. The resulting crystals were collected by filtration and dried in vacuum cabinet to yield the title compound, 0.92 g (66%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09439904B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-f83ca43a663a4b1dbcd984fadc2d0142 |
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| 出典メモ | uspto-grants-2016_09 |
|---|