化工社化工社 化学情報印刷レポート · 研究参考用
Methylamine → 6-chloro-N4-methylpyrimidine-4,5-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Amino-4,6-dichloropyrimidine | HCID 79434 | — |
| 生成物 | 6-chloro-N4-methylpyrimidine-4,5-diamine | HCID 308477 | — |
反応手順
5-Amino-4,6-dichloropyrimidine (15.0 g, 91.4 mmol) and methylamine (2M solution in THF, 5 eq) were initially charged, and triethylamine (27.76 g, 274 mmol) was added. The mixture was stirred under reflux until the conversion was complete (about 3 hours). The reaction mixture was then concentrated, and water was added to the residue. The pH was adjusted to 7-8 using saturated Na—HCO3 solution. The mixture was extracted 3× with methylene chloride, the combined organic phases were dried over sodium sulphate and filtered and the solvent was removed under reduced pressure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08202877B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-1b3c0f54b6a64ce092d07c822d9f1de4 |
| 出典メモ | uspto-grants-2012_06 |