反应 #69965

反应方程式

4-chloro-5-methyl-2-methylsulfanylpyrimidine

10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione

X-Phos

potassium phosphate

→

4-(5-methyl-2-methylsulfanyl-pyrimidin-4-yl)-10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione

收率 11.2%

溶剂

1,2-dimethoxyethane

反应条件

后处理

1. 1
   workup.ADDITIONSilica gel is added to the crude
2. 2
   其他reaction mixture
3. 3
   其他the solvent is evaporated under reduced pressure
4. 4
   其他the residue is purified by flash chromatography on silica gel

实验过程

A microwave vial is charged with 4-chloro-5-methyl-2-methylsulfanylpyrimidine (174 mg, 1 mmol), 10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (166 mg, 1 mmol), palladium acetate (12 mg, 0.05 mmol), X-Phos (48 mg, 0.1 mmol) and potassium phosphate (424 mg, 2 mmol). 1,2-dimethoxyethane (3 ml) is added and the reaction heated to 160° C., with stirring, for 30 minutes. Silica gel is added to the crude reaction mixture, the solvent is evaporated under reduced pressure and the residue is purified by flash chromatography on silica gel to give 4-(5-methyl-2-methylsulfanyl-pyrimidin-4-yl)-10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (34 mg).

来源