4,6-Dichloro-2-(methylthio)pyrimidine → 4-Chloro-6-methyl-2-(methylthio)pyrimidine
反応式
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.[CH3:11][Mg+].[Br-]>C1COCC1>[Cl:1][C:2]1[CH:7]=[C:6]([CH3:11])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1参加物
4
実験手順
According to Scheme 12, a solution of 4,6-dichloro-2-methylthiopyrimidine (1.95 g, 10 mmol) in 30 mL of dry THF was cooled to 0° C. and treated with a solution of MeMgBr (14 mL of 1.4 M solution, 19.6 mmol). After overnight stirring at RT, the reaction mixture was quenched with sat. NH4Cl. The organic layer washed with brine, dried and evaporated. The residue was purified by chromatography (silica gel, hexane:ethyl acetate, 9:1) to provide 1.3 g of 4-chloro-6-methyl-2-methylthiopyrimidine (95).
後処理
- customthe reaction mixture was quenched with sat. NH4Cl
- washThe organic layer washed with brine
- customdried
- customevaporated
- customThe residue was purified by chromatography (silica gel, hexane:ethyl acetate, 9:1)
出典と根拠
- ORDレコード
- ord-aa26f250983441a38aa20a57ec12143b
- 出典データセット
- uspto-grants-2005_07
- 特許番号
- US06919347B2
反応ノート
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