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Methanesulfonic Acid → 2-(4-Carboxypiperidino)-4-(3,4-methylenedioxy-benzyl)amino-6-chloroquinazoline methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 1-(6-Chloro-4-(3,4-methylenedioxybenzyl)aminoquinazolin-2-yl)piperidine-4-carboxylic acid | HCID 5311486 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(4-Carboxypiperidino)-4-(3,4-methylenedioxy-benzyl)amino-6-chloroquinazoline methanesulfonate | HCID 21184032 | 90.7% |
反応手順
2.00 g (4.54 mmol) of the 2-(4-carboxypiperidino)-4-(3,4-methylenedioxybenzylamino)-6-chloroquinazoline prepared in Example 222 was dissolved in a mixture comprising 25 ml of tetrahydrofuran and 25 ml of ethanol under heating, followed by the dropwise addition of 0.31 ml (4.78 mmol) of methanesulfonic acid. The obtained mixture was cooled by allowing to stand to precipitate crystals. The crystals were recovered by filtration, washed with tetrahydrofuran, and air-dried to give 2.21 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05576322 |
| 出典データセット | uspto-grants-1996_11 |
| ORD ID | ord-fbef7d8271504b808e6dc10516fe6b79 |
| 出典メモ | uspto-grants-1996_11 |