関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Propyl Gallate | HCID 4947 | — |
| 反応物 | Methyl piperazine-1-carbodithioate | HCID 21278808 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Methyl 4-(6-propyloxycarbonyl-2,3,4-trihydroxybenzyl)-1-piperazinecarbodithioate | HCID 53992097 | 46.1% |
反応手順
In 10 ml of ethanol was dissolved 0.86 g (10 mmol.) of 35% formalin. To thesolution placed in an ice bath was further added a solution of 1.94 g (10 mmol., purity 90.7%) of methyl 1-piperazinecarbodithioate in 4 ml of ethanol. The resulting mixture was then stirred for 30 min. at room temperature. To the mixture placed in an ice bath was dropwise added a solution of 2.12 g (10 mmol.) of propyl gallate in 4 ml of ethanol. The mixture was stirred overnight at room temperature and subsequently refluxed under heating for 4 hours. The mixture was cooled to room temperature. Precipitated crystals were collected by filtration and washedwith ethanol to give 1.848 g of the desired compound as a grayish powder, m.p. 142°-144° C. (decomp.), yield 31.3%.
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-add8c06a27be4b73877e44f6eb09ab5a |
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| 出典メモ | uspto-grants-1995_08 |
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