化工社化工社 化学情報印刷レポート · 研究参考用
3,4,5-Trimethoxyphenyl isothiocyanate → 4-(3-Chlorophenyl)-1-(3-[3,4,5-trimethoxyphenyl(thiocarbamoyl)oxy]propyl)piperazine, hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,4,5-Trimethoxyphenyl isothiocyanate | HCID 118900 | — |
| 反応物 | 3-(4-(3-Chlorophenyl)piperazin-1-yl)propan-1-ol | HCID 257407 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-(3-Chlorophenyl)-1-(3-[3,4,5-trimethoxyphenyl(thiocarbamoyl)oxy]propyl)piperazine, hydrochloride | HCID 131718165 | 38.7% |
反応手順
A mixture of 3,4,5-trimethoxyphenylisothiocyanate (2.0 mmol) (produced as in Example 22) and 3-[4-(3-chlorophenyl) -1-piperazinyl]propanol (510 mg; 2.0 mmol) in toluene (40 ml) was refluxed for 16 h. The solvent was evaporated and the residue resuspended in ethyl acetate, filtered and evaporated to dryness. The residue was submitted to flash chromatography on silica gel 60 eluting with toluene/ethyl acetate (1:1). The product was taken up in ethanol, which was treated with hydrogen chloride in ether to give 200 mg of the title compound. M.p. 175°-176° C. MS (70 eV): m/z 479 (M+, 0.5%), 254 (49), 225 (88), 209 (100), 182 (34).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246935 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-32f0e1a47d884b0fa22a2aeb54b8e2e5 |
| 出典メモ | uspto-grants-1993_09 |