4,6-Dichloro-2-(methylthio)pyrimidine → 4-Chloro-6-methyl-2-(methylthio)pyrimidine
반응식
[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]=1참가 물질
4
실험 절차
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).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-aa26f250983441a38aa20a57ec12143b
- 출처 데이터셋
- uspto-grants-2005_07
- 특허 번호
- US06919347B2
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