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2,4'-Dichloroacetophenone → 2-(4-Chlorophenyl)-2-oxoethyl thiocyanate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,4'-Dichloroacetophenone | HCID 70298 | — |
| 反応物 | Potassium thiocyanate | HCID 516872 | — |
| 生成物 | 2-(4-Chlorophenyl)-2-oxoethyl thiocyanate | HCID 88013 | 90% |
反応手順
A solution of 945 mg (5 mmol) 2,4′-dichloroacetophenone and 583 mg (6 mmol) potassium rhodanide was heated to reflux for 30 minutes. After a few minutes a precipitation was formed. The solvent was evaporated under reduced pressure and the residue was suspended in tetrahydrofurane, stirred for 1 hour at room temperature, filtered and the filtrate was concentrated in vacuo. The residue was stirred with heptane and little ethanol for 15 minutes. The product was filtered off and dried to yield 953 mg (90%) 1-(4-chloro-phenyl)-2-thiocyanato-ethanone as a light yellow solid. 1H NMR (CDCl3, 250 MHz): δ (ppm)=7.89 (d, 2H), 7.51 (d, 2H), 4.692 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07910740B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-f236601bf5e449eeadf020241375a1af |
| 出典メモ | uspto-grants-2011_03 |