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Chlorosuccinimide → 5-chloro-6-ethyl-2-phenyl-4(3H)-pyrimidinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | 6-Ethyl-2-phenylpyrimidin-4(1H)-one | HCID 135629822 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-chloro-6-ethyl-2-phenyl-4(3H)-pyrimidinone | HCID 135837536 | 87.1% |
反応手順
A stirred solution of 7.81 g (39.1 mmol) of 6-ethyl-2-phenyl-4(3H)-pyrimidinone and 5.80 g (43.4 mmol) of N-chlorosuccinimide in 100 mL of glacial acetic acid was heated at 90° C. for 4 h. The mixture was cooled, poured onto crushed ice and allowed to stand until the ice had melted. The mixture was filtered and the solid collected was washed with water and a little ether. The solid was dried in a vacuum oven at 50C to afford 7.99 g of 5-chloro-6-ethyl-2-phenyl-4(3H)-pyrimidinone (an intermediate for compound 172) as a white solid. 1H-NMR (d6-DMSO) 1.30(3H,t), 2.8(2H,q), 7.6(3H,m), 8.2(2H.m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726124 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-475d4575be964743a02cc9754560986f |
| 出典メモ | uspto-grants-1998_03 |