Phosphorus oxychloride → 4-Chloro-6-methyl-2-(methylthio)pyrimidine
反応式
O[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.P(Cl)(Cl)([Cl:13])=O>>[Cl:13][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1参加物
3
実験手順
4-Hydroxy-6-methyl-2-(methylthio)pyrimidine (9.20 g, 59 mmol) and phosphorous oxychloride (60 mL) were combined and refluxed for 3 hours. The reaction mixture was cooled to room temperature and poured onto crushed ice. The resultant aqueous mixture was extracted with ethyl acetate; and the organic layer washed with saturated aqueous sodium bicarbonate followed by a water wash, dried over magnesium sulfate, and dried in vacuo to give 4-chloro-6-methyl-2-(methylthio)pyrimidine (8.27 g, 80%), m.p. 37°-38° C.
後処理
- temperaturerefluxed for 3 hours
- additionpoured
- customonto crushed ice
- extractionThe resultant aqueous mixture was extracted with ethyl acetate
- washand the organic layer washed with saturated aqueous sodium bicarbonate
- washwash
- dry with materialdried over magnesium sulfate
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-98a5dd7fdda34899b5a9b85033b0fa91
- 出典データセット
- uspto-grants-1999_01
- 特許番号
- US05863924
反応ノート
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