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Water → 3-Phenyl-2-[(4-methylpyridin-2-yl)methylthio]-4(3H)-quinazolinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 2-(Chloromethyl)-4-methylpyridine hydrochloride | HCID 20061071 | — |
| 反応物 | HCID 178515047 | HCID 178515047 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Phenyl-2-[(4-methylpyridin-2-yl)methylthio]-4(3H)-quinazolinone | HCID 14575169 | 30.7% |
反応手順
8.7 ml of 28% methanolic solution of sodium methoxide were added to a solution of 5.0 g of 2-mercapto-3-phenyl-4(3H)-quinazolinone and 4.0 g of 2-chloromethyl-4-methylpyridine hydrochloride in methanol, and the stirring was continued at room temperature for 5 hours. The reaction solution was poured into water and extracted with chloroform. The chloroform layer was washed with an aqueous solution of sodium carbonate and dried over sodium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography. The fraction eluted with 8% ethyl acetate in chloroform was collected and crystallized from ethyl acetate to give 2.17 g (30.7%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05008266 |
| 出典データセット | uspto-grants-1991_04 |
| ORD ID | ord-650ced8df29c4ed4af120a116f7fb3c1 |
| 出典メモ | uspto-grants-1991_04 |