m-Chloroperbenzoic acid → 2,4-Dichloro-3,6-dimethylpyridine 1-oxide
반응식
[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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-032444b1fbe0455695a20821715e07e8
- 출처 데이터셋
- uspto-grants-2005_10
- 특허 번호
- US06956047B1
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