関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 2,3,4-Trimethoxyphenylacetic acid | HCID 89727 | — |
| 反応物 | Methyl piperazine-1-carbodithioate | HCID 21278808 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 4-(2,3,4-trimethoxyphenylacetyl)-1-piperazinecarbodithioate | HCID 19388512 | 48.8% |
反応手順
In 6.2 ml of methylene chloride were dissolved 310 mg (1.37 mmol.) of 2,3,4-trimethoxyphenylacetic acid and 289 mg (1.64 mmol.) of methyl 1-piperazinecarbodithioate. To the solution was added 395 mg (1.92 mmol.) of dicyclohexylcarbodiimide. The mixture was stirred at room temperature for 1 hour. A precipitated solid was removed by filtration, and to the filtrate were added methylene chloride and 1-N hydrochloric acid. The organic solvent potitoh was taken out, washed with a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and placed under reduced pressure to distill off the solvent. The residue was purified over a silica gel column. The obtained oil was crystallized from a mixture of ethanol and hexane, yielding 257 mg of the desired compound as a white crystalline product, m.p. 119°-120° C., yield 48.8%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05446146 |
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| 出典データセット | uspto-grants-1995_08 |
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| ORD ID | ord-68e23283115649c09ec2f10ba42e7617 |
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| 出典メモ | uspto-grants-1995_08 |
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