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Butyryl chloride → (+)-2-(4-(3-Butyryloxy-4,4,4-trifluoro-1-butenyl)phenyl)-5-decyloxypyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Butyryl chloride | HCID 8855 | — |
| 反応物 | (-)-2-(4-(3-Hydroxy-4,4,4-trifluoro-1-butenyl)phenyl)-5-decyloxypyrimidine | HCID 54106197 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (+)-2-(4-(3-Butyryloxy-4,4,4-trifluoro-1-butenyl)phenyl)-5-decyloxypyrimidine | HCID 54507690 | 93.1% |
反応手順
1.0 g of (-)-2-(4-(3-hydroxy-4,4,4-trifluoro-1-butenyl) phenyl)-5-decyloxypyrimidine was dissolved in 20 ml of pyridine. The solution was added with 0.5 g of butyryl chloride and stirred at 25°-30° C. for 4 hours. The reaction mixture was diluted with 100 ml of toluene and washed with 4N hydrochloric acid, water, a 5% sodium bicarbonate solution and water successively in that order, and then the toluene layer was concentrated under reduced pressure. The residue was purified by subjecting it to silica gel column chromatography using toluene/ethyl acetate as eluent to obtain 1.08 g of (+)-2-(4-(3-butyryloxy-4,4,4-trifluoro-1-butenyl) phenyl)-5-decyloxy-pyrimidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723610 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-a527bf234aeb411088cf0a7588b93b15 |
| 出典メモ | uspto-grants-1998_03 |