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2,5-Diamino-4,6-dichloropyrimidine → HCID 178496608、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,5-Diamino-4,6-dichloropyrimidine | HCID 301039 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | HCID 178496609 | HCID 178496609 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | HCID 178496608 | HCID 178496608 | 69% |
反応手順
2,5-diamino-4,6-dichloropyrimidine (6 g, 33.5 mmol), trans-4-methoxy cyclohexyl amine (4.32 g, 33.5 mmol, 1 equiv.), sodium bicarbonate (9.85 g, 117.2 mmol, 3.5 equiv.) and 1-butanol (350 mL) were heated together at 150° C. in a sealed tube. After 3 days, when the reaction appeared to be complete (by HPLC), the reaction mixture was cooled to room temperature and the solvent was removed in vacuo. The residue was purified by flash chromatography (silica gel, gradual elution with 96/4 methylene chloride/methanol to 90/10 methylene chloride/methanol) to give the desired product as a brown solid (69% yield). MS (EI) m/z 272 (MH)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07902187B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-7e27267da80c485eb475144a3183b98d |
| 出典メモ | uspto-grants-2011_03 |