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Methyl Methanesulfonate → 1-(2-Hydroxyethyl)-2-methylthio-3,4,5,6-tetrahydropyrimidine mesylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Methanesulfonate | HCID 4156 | — |
| 反応物 | 1-(2-Hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione | HCID 3603281 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 1-(2-Hydroxyethyl)-2-methylthio-3,4,5,6-tetrahydropyrimidine mesylate | HCID 86747344 | 128.8% |
反応手順
Then, 1-(2-hydroxyethyl)-3,4,5,6-tetrahydropyrimidine-2-thione (121.2 g) and methyl methanesulfonate (91.51 g) are heated at reflux in ethyl alcohol (200 ml) for about 2 hours and then allowed to cool to room temperature. The mixture was diluted with t-butyl methyl ether (2 liters). An oil separates which crystallizes on keeping in freezer at -20° C. Filtration and drying yields 145.7 g of 1-(2-hydroxyethyl)-2-methylthio-3,4,5,6-tetrahydropyrimidine mesylate, melting point 61.7°-62.2° 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-333625bfe3524323baec2a941c41e1f7 |
| 出典メモ | uspto-grants-1993_11 |