化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 1,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Ethyl trifluoroacetate | HCID 9794 | — |
| 反応物 | 1-(4-(Methylthio)phenyl)ethan-1-one | HCID 74501 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 1,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]- | HCID 10730170 | 71% |
反応手順
To a solution of ethyl trifluoroacetate (7.95 ml, 1.1 eq) in MTBE (125 ml) was added dropwise 25% sodium methoxide in methanol (16 ml, 1.2 eq). 4-Methylthioacetophenone (Aldrich, 10 g, 0.06 mol) was added portionwise and the mixture stirred at ambient temperature overnight. 2N Hydrochloric acid (40 ml) was added cautiously and the organic phase separated, washed with brine and dried (Na2SO4) to give an orange solid. The orange solid was recrystallised from hot isopropanol to give the title compound as a yellow crystalline solid (11.25 g, 71%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084148B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-697eb1beb35a4059a73112f3071f16a1 |
| 出典メモ | uspto-grants-2006_08 |