化工社化工社 化学情報印刷レポート · 研究参考用
Water → 9-[4-(1-Methylethoxy)phenyl]-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethanesulfonylchloride, 2-chloro- | HCID 15385 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-(4-Isopropoxyphenyl)pyridin-2-amine | HCID 64087698 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 9-[4-(1-Methylethoxy)phenyl]-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide | HCID 66747896 | 73.7% |
反応手順
A mixture of 3-[4-(1-methylethoxy)phenyl]pyridin-2-amine (350 mg) in dehydrated THF (5 mL) was added to a mixture of sodium hydride (60%, 307 mg) and 2-chloroethanesulfonyl chloride (750 mg) in dehydrated THF (5 mL) under ice-cooling. The reaction mixture was stirred at room temperature overnight, and water and hexane were added. The resulting precipitate was collected by filtration, and washed with water and diisopropyl ether to give the title compound (360 mg) as a white solid. The obtained solid was crystallized from THF, acetonitrile and diisopropyl ether to give a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08916551B2 |
| 出典データセット | uspto-grants-2014_12 |
| ORD ID | ord-195860de6ce74c33b44581e316ce6253 |
| 出典メモ | uspto-grants-2014_12 |