Potassium Persulfate → 4,6-Dichloropyrimidine-5-carboxylic acid
반응식
[Cl:1][C:2]1[C:7]([CH:8]=[O:9])=[C:6]([Cl:10])[N:5]=[CH:4][N:3]=1.S(OOS([O-])(=O)=O)([O-])(=O)=[O:12].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[C:7]([C:8]([OH:12])=[O:9])=[C:6]([Cl:10])[N:5]=[CH:4][N:3]=1참가 물질
4
실험 절차
A solution of 4,6-dichloro-5-pyrimidinecarbaldehyde (15.0 g, 84.8 mmol) in DMF (360 mL) was charged with potassium monopersulfate (38.9 g, 254 mmol) and stirred over night at rt. The reaction mixture was filtered through a pad of celite and partitioned between EtOAc and water and separated. The aqueous was extracted with EtOAc (3×) and the combined organic fractions were washed with water (2×), brine, and dried over sodium sulfate, filtered, and concentrated to afford the title compound. 1H NMR (DMSO-d6, 400 MHz): δ=9.02 (s, 1H).
후처리
- filtrationThe reaction mixture was filtered through a pad of celite
- custompartitioned between EtOAc and water
- customseparated
- extractionThe aqueous was extracted with EtOAc (3×)
- washthe combined organic fractions were washed with water (2×), brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-43f44a3109d24948a651be92b5c5b4ae
- 출처 데이터셋
- uspto-grants-2013_03
- 특허 번호
- US08399433B2
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