m-Chloroperbenzoic acid → 2,4-Dichloro-3,6-dimethylpyridine 1-oxide
反応式
[Cl:1][C:2]1[C:7]([CH3:8])=[C:6]([Cl:9])[CH:5]=[C:4]([CH3:10])[N:3]=1.ClC1C=CC=C(C(OO)=[O:19])C=1>C(Cl)(Cl)Cl>[Cl:1][C:2]1[C:7]([CH3:8])=[C:6]([Cl:9])[CH:5]=[C:4]([CH3:10])[N+:3]=1[O-:19]参加物
4
実験手順
A mixture of 2,4-dichloro-3,6-dimethyl-pyridine (790 mg, 4.49 mmol) and 50% m-chloro-perbenzoic acid (1.544 g, 4.49 mmol) in 10 ml of chloroform was stirred at room temperature for 20 hours. The mixture was quenched with water, washed with saturated sodium thiosulfate and saturated sodium carbonate, brine and extracted with chloroform. The organic layer was dried and concentrated to give 954 mg of crude material. The material was purified through silica gel to give 662 mg of the title compound as a white crystals, mp 131-132° C. 1H NMR (CDCl3) δ 7.22 (s, 1H), 2.51 (s, 3H), 2.47 (s, 3H) ppm.
後処理
- customThe mixture was quenched with water
- washwashed with saturated sodium thiosulfate and saturated sodium carbonate, brine
- extractionextracted with chloroform
- customThe organic layer was dried
- concentrationconcentrated
- customto give 954 mg of crude material
- customThe material was purified through silica gel
出典と根拠
- ORDレコード
- ord-032444b1fbe0455695a20821715e07e8
- 出典データセット
- uspto-grants-2005_10
- 特許番号
- US06956047B1
反応ノート
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