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Hydrochloric Acid → 1-(2-Hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Carbon Disulfide | HCID 6348 | — |
| 反応物 | N-(Aminopropyl)ethanolamine | HCID 78211 | — |
| 溶媒 | Water ethanol | HCID 19096565 | — |
| 生成物 | 1-(2-Hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione | HCID 3603281 | — |
反応手順
2-(3-Aminopropylamino)ethanol (118 ml) is dissolved in 1:1 ethyl alcohol-water (340 ml) and heated to 40°-50° C. Carbon disulfide (60 ml) is added dropwise over a period of about 15 minutes. An exothermic reaction occurs after about half of the amount of carbon disulfide is added. After the addition of all the carbon disulfide, the mixture is refluxed for about 1 hour. Concentrated hydrochloric acid (8 ml) is then added, and the reaction mixture is refluxed overnight. After cooling in an ice bath, the crystalline solid which separates is filtered, washed with isopropyl alcohol and t-butyl methyl ether, and dried to give 129-4 g of 1-(2-hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione, melting point 112°-114° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05258381 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-4d01249e829942b499b83f7e31d5cabb |
| 出典メモ | uspto-grants-1993_11 |