Thiophenol → 2-Chloro-4-(phenylthio)pyrimidine
반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.[Na].[C:10]1([SH:16])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C(O)C.C(OCC)(=O)C>[Cl:1][C:2]1[N:7]=[C:6]([S:16][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:5]=[CH:4][N:3]=1참가 물질
6
실험 절차
To a stirred solution of 2,4-dichloropyrimidine (1.00 g, 6.71 mmol) in absolute ethanol (10 mL), was added sodium salt of benzenethiol (0.89 g, 6.73 mmol)in small portions. The mixture was stirred at room temperature for 2 hours, then at 40° C. for 16 hours. It was diluted with ethyl acetate (20 mL), and filtered. The filtrate was concentrated in vacuo, and the residue was flash chromatographed on silica gel using ethyl acetate:petroleum ether (1:99→25:75) as eluant to give the desired product (498 mg, 36%).
후처리
- waitat 40° C. for 16 hours
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo
- customchromatographed on silica gel
출처 및 근거
- ORD 기록
- ord-3ed04ce3ef9b4af6adf98607be7aa7e5
- 출처 데이터셋
- uspto-grants-2015_05
- 특허 번호
- US09040549B2
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