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Ethanesulfonylchloride, 2-chloro- → 9-[4-(3-Methoxyphenoxy)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-(3-Methoxyphenoxy)phenyl)pyridin-2-amine | HCID 66748860 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9-[4-(3-Methoxyphenoxy)phenyl]-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide | HCID 66749342 | — |
反応手順
To a suspension of NaH (60%, 143 mg) in THF (dry) (15 mL) was added 2-chloroethanesulfonyl chloride (0.376 mL) at 0° C. and the mixture was stirred for 5 min at the same temperature. A solution of 3-(4-(3-methoxyphenoxy)phenyl)pyridin-2-amine (348 mg) in THF (dry) (15 mL) was added at 0° C. and the mixture was stirred at room temperature under nitrogen for 15 hr. The mixture was quenched with water at 0° C. carefully and water was added to form precipitates. The precipitate was crystallized from MeCN-THF-MeOH/IPE to give the title compound (304 mg) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08778934B2 |
| 出典データセット | uspto-grants-2014_07 |
| ORD ID | ord-ae4e60567e814bd5a38647d4978f0013 |
| 出典メモ | uspto-grants-2014_07 |