化工社化工社 化学情報印刷レポート · 研究参考用
Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)- → Cyclopentyl-(5-[(2,6-difluoro-3,5-dimethoxy-phenylimino)-methyl]-2-methylsulfanyl-pyrimidin-4-yl)-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)- | HCID 18462 | — |
| 反応物 | 2,6-Difluoro-3,5-dimethoxybenzenamine | HCID 10261892 | — |
| 反応物 | 4-(Cyclopentylamino)-2-(methylthio)pyrimidine-5-carbaldehyde | HCID 10799896 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Cyclopentyl-(5-[(2,6-difluoro-3,5-dimethoxy-phenylimino)-methyl]-2-methylsulfanyl-pyrimidin-4-yl)-amine | HCID 18444836 | — |
反応手順
In a 1-L round bottom flask, 10.00 g (0.0528 mol) of 2,6-difluoro-3,5-dimethoxy-phenylamine and 12.42 g (0.0523 mol) of 4-cyclopentylamino-2-methylsulfanyl-pyrimidine-5-carbaldehyde in 500 mL of toluene with 3.65 g (0.0157 mol) of camphorsulfonic acid was fitted with a Dean Stark trap and heated at reflux. During the day, the toluene was drained three times from the finger and continued heating at reflux under nitrogen atmosphere overnight. The toluene was concentrated in vacuo and dried to give 25.30 g (quantitative) of the title compound. No further purification was necessary. MS (APCI) (m+1)/z 409.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07196090B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-2eeebb61abd64651bda7230d69a15e8d |
| 出典メモ | uspto-grants-2007_03 |