تفاعل #69965

معادلة التفاعل

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

المردود 11.2%

المذيبات

1,2-dimethoxyethane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر