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m-Chloroperbenzoic acid → 5-Bromo-2-chloro-4-methylpyridine 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 5-Bromo-2-chloro-4-methylpyridine | HCID 2734427 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 5-Bromo-2-chloro-4-methylpyridine 1-oxide | HCID 86652346 | — |
反応手順
A solution of 5-bromo-2-chloro-4-methylpyridine (1.0 eq.) and meta-chloroperbenzoic acid (mCPBA) (2.5 eq.) in chloroform (0.1 M) was stirred at 50° C. overnight. After cooling to room temperature, Ca(OH)2 (2.5 eq.) was added to the reaction mixture. The precipitate was filtered and washed with 5% methanol in dichloromethane and ethyl acetate. The filtrate was washed with saturated aqueous Na2S2O3 solution and saturated aqueous NaHCO3 solution. The combined organic layers were washed with brine, dried over anhydrous MgSO4, and concentrated en vacuo into a pale solid that was carried onto the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895577B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-1baaecbc62394e599a729f9073c99271 |
| 出典メモ | uspto-grants-2014_11 |