関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperazine, 1-(1-adamantyl)- | HCID 35373 | — |
| 反応物 | 2,4-Diamino-6-chloropyrimidine | HCID 67432 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(1-Adamantyl)-4-(2,6-diamino-4-pyrimidinyl)-piperazine | HCID 18946300 | 80.2% |
反応手順
A mixture of 2,6-diamino-4-chloropyrimidine (0.43 g, 3.0 mmol) and 1-(1-adamantyl)-piperazine (0.66 g, 3.0 mmol) in ethanol (30 ml) was heated in a sealed tube at 170° C. for 3 hours. After cooling the solvent was removed, the solid residue was dissolved in water (45 ml) and acidified to pH=3 with conc. HCl. The obtained mixture was heated to 50° C. the insolubles were filtered off and the clear solution was rendered alkaline with 10N NaOH under stirring and cooling. The precipitated crystals were collected, washed with water until neutral and dried. In this manner 0.79 g of the title compound was obtained in the form of its monohydrate, yield: 76.6%, mp. 265°-268° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05380724 |
|---|
| 出典データセット | uspto-grants-1995_01 |
|---|
| ORD ID | ord-ffaac1866e2e41fd8560fdae32cb8b29 |
|---|
| 出典メモ | uspto-grants-1995_01 |
|---|