化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Carbonate → 2-[1-(4-Amino-6,7,8-trimethoxy-2-quinazolinyl)-4-piperidinyl]-isoindolin-1-one monohydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Chloro-6,7,8-trimethoxyquinazolin-4-amine | HCID 3015804 | — |
| 反応物 | 2-(Piperidin-4-yl)isoindolin-1-one | HCID 15431961 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[1-(4-Amino-6,7,8-trimethoxy-2-quinazolinyl)-4-piperidinyl]-isoindolin-1-one monohydrochloride | HCID 20556249 | — |
反応手順
The mixture of 5.39 g of 4-amino-2-chloro-6,7,8-trimethoxy-quinazoline, 4.32 g of 2-(4-piperidinyl)-isoindolin-1-one, 4.24 g of anhydrous sodium carbonate and 75 ml of dimethylformamide is stirred under nitrogen at 125°-130° for 16 hours. It is filtered, the filtrate evaporated, the residue dissolved in methylene chloride and the solution washed with aqueous sodium bicarbonate. The organic layer is separated, dried, and evaporated. The residue is suspended in refluxing isopropanol and acidified with hydrogen chloride to pH=1. The precipitate formed is filtered off and triturated with warm ethanol to yield the 2-[1-(4-amino-6,7,8-trimethoxy-2-quinazolinyl)-4-piperidinyl]-isoindolin-1-one monohydrochloride melting at 234° (dec.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04255429 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-faf9295f48a842a48eb8a5dd0b9cfae3 |
| 出典メモ | uspto-grants-1981_03 |