Thiophenol → 2-Chloro-4-(phenylthio)pyrimidine
反応式
[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]=1参加物
6
実験手順
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%).
後処理
- waitat 40° C. for 16 hours
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo
- customchromatographed on silica gel
出典と根拠
- ORDレコード
- ord-98a58531368e4b3a9fc71ff718e59e4b
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846704B2
反応ノート
読み込み中…