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Hydrazine → 4-Hydrazinyl-2-(methylthio)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine | HCID 9321 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Chloro-2-methylthiopyrimidine | HCID 97113 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Hydrazinyl-2-(methylthio)pyrimidine | HCID 13590472 | 57.6% |
反応手順
In a 250 mL round bottom flask, 4-chloro-2-methylsulfanyl-pyrimidine (5 g, 31.1 mmol), hydrazine (4.5 g, 140 mmol) and potassium carbonate (6.45 g, 46.7 mmol) were combined with ethanol (50 mL). The mixture was refluxed for 3 hrs and filtered. The filtered solid was rinsed with ethanol (30 mL). The combined ethanol solution was evaporated to give a crude oily mixture which was purified by ISCO flash column chromatography (30% to 100% ethyl acetate in hexanes) to give N-(2-methylsulfanyl-pyrimidin-4-yl)-hydrazine as a white solid (2.8 g, 57.6% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536172B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-55ba855f3dbe488fa50adf6929cf0b03 |
| 出典メモ | uspto-grants-2013_09 |