反応 #69965

反応方程式

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

収率 11.2%

溶媒

1,2-dimethoxyethane

反応条件

後処理

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

実験手順

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).

出典