化工社化工社 化学情報印刷レポート · 研究参考用
Ethanesulfonylchloride, 2-chloro- → 9-(4-((Tert-butyl(dimethyl)silyl)oxy)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 | Ethanesulfonylchloride, 2-chloro- | HCID 15385 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-(4-((Tert-butyl(dimethyl)silyl)oxy)phenyl)pyridin-2-amine | HCID 66747707 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9-(4-((Tert-butyl(dimethyl)silyl)oxy)phenyl)-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide | HCID 66747725 | — |
反応手順
To a suspension of NaH (60%, 42.0 g) in THF (dry) (350 mL) was added 2-chloroethanesulfonyl chloride (44.5 mL) at 0° C. and the mixture was stirred for 10 min at the same temperature. A solution of 3-(4-((tert-butyl(dimethyl)silyl)oxy)phenyl)pyridin-2-amine (78.8 g) in THF (dry) (350 mL) was added at 0° C. and the mixture was stirred at room temperature under N2 overnight. The mixture was quenched with water at 0° C. carefully. Additional water was added to form precipitates which were washed with water and EtOAc and collected to give the title compound (65.5 g) as an off-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-8a959c2b3a22499481ffd73787831205 |
| 出典メモ | uspto-grants-2014_12 |