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Water → Acetanilide, 3'-acetyl-2,2,2-trifluoro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3'-Aminoacetophenone | HCID 7417 | — |
| 反応物 | Methyl trifluoroacetate | HCID 9893 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Acetanilide, 3'-acetyl-2,2,2-trifluoro- | HCID 673706 | 85% |
反応手順
10 mmol of 3′-aminoacetophenone as a starting material was dissolved in a methanol solvent in a 100 mL round-bottomed flask and 1.2 equivalents (eq) of methyl trifluoroacetate was added dropwise thereto over 30 minutes at room temperature, and subsequently the reaction mixture was stirred for 2 hours. After the completion of the reaction was confirmed by TLC, a small amount of water was added to terminate the reaction. Then, the solvent was removed under reduced pressure. The residue was dissolved in 50 mL of ethyl acetate and washed twice with 30 mL of water, dried over anhydrous sodium sulfate, and distilled under reduced pressure to obtain the desired 3-acetyl-trifluoroacetylaminobenzene (85%) as a brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07566773B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-765ccfd9ba554e248b48d58848b357ce |
| 出典メモ | uspto-grants-2009_07 |