関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (Phenylthio)acetic acid | HCID 59541 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | 2-Bromo-4'-(methylsulfonyl)acetophenone | HCID 735823 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-Phenylthio-4-(4-(methylsulfonyl)phenyl)-5h-furan-2-one | HCID 10269135 | — |
反応手順
At 0° C., triethylamine (335 μL) was added to a solution of thiophenoxyacetic acid (161 mg) and 2-bromo-l-(4-(methylsulfonyl) phenyl) ethanone (272 mg, WO 9500501, example 9, Step 1) in 5 mL of acetonitrile and the mixture was stirred at 0° C. for 1 h. The reaction mixture was then cooled to -20° C. and DBU (265 μL) was added. The mixture was stirred for 30 min. at -20° C. and was quenched by addition of 1N HCl. The product was extracted with EtOAc, dried over sodium sulfate and partially purified by silica gel chromatography. The impure product was recrystalized from EtOAc/Hexane to afford the title compound as a solid
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05789413 |
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| 出典データセット | uspto-grants-1998_08 |
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| ORD ID | ord-6197c4ee24984d6da99e2e74b559676a |
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| 出典メモ | uspto-grants-1998_08 |
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