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Acetoin → (+/-)-3-(4,6-Dimethoxy-2-pyrimidinyloxy)-2-butanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetoin | HCID 179 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium methanesulfinate | HCID 2733271 | — |
| 反応物 | 2-Chloro-4,6-dimethoxypyrimidine | HCID 5152323 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (+/-)-3-(4,6-Dimethoxy-2-pyrimidinyloxy)-2-butanone | HCID 15526619 | — |
反応手順
4.38 g (25 mmol) of 2-chloro-4,6-dimethoxypyrimidine, 2.31 g (26.2 mmol) of 3-hydroxy-2-oxobutane and 0.66 g (6.3 mmol) of sodium methanesulfinate were heated in the presence of 5.17 g (37.5 mmol) of potassium carbonate in 25 ml of N,N-dimethylformamide to 120° C. with stirring. After 3 hours, the solvent was removed in a rotary evaporator at 70° C./20 mbar. The residue was purified by chromatography on a silica gel column (eluent hexane/ethyl acetate 4:1). The title product was obtained from the product fraction in the form of a pale yellowish oil in a yield of 4.58 g (80.4 percent of theory) (GC content 99 percent). Other data concerning the title compound was:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05840892 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-7528507575514fc1b1849363e5f6023b |
| 出典メモ | uspto-grants-1998_11 |