反応式
[OH-].[Na+].Cl.[CH3:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([SH:11])[N:6]=1.I[CH3:13]>O>[CH3:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([S:11][CH3:13])[N:6]=1参加物
5
実験手順
To a solution of NaOH (7.46 g, 186.4 mmol) in water (120 mL), 4-methylpyrimidine-2-thiol hydrochloride (13.78 g, 84.7 mmol) was added and subsequently iodomethane (13.23 g, 93.2 mmol) was added dropwise under argon atmosphere. It was stirred at room temperature for 2 h. It was extracted with CH2Cl2 (×2). The organic phase was dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford 10.26 g of the desired compound (yield: 86%).
後処理
- extractionIt was extracted with CH2Cl2 (×2)
- dry with materialThe organic phase was dried over Na2SO4
- concentrationconcentrated to dryness
- customThe crude product obtained
- customwas purified by chromatography on silica gel
- temperatureof increasing polarity as eluent
出典と根拠
- ORDレコード
- ord-28d9962299d84e278f896f2ad27afb03
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08536194B2
関連ノート
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