反应详情

To 0.10 mole of phenyl lithium in 100 ml. of benzene/ether at 0°C. is added dropwise 10.6 g. (0.084 mole) of 2-(methoxymethyl)pyridine dissolved in 75 ml. of benzene. To this mixture is added dropwise 10.0 g. (0.081 mole) of N,N-dimethylthiocarbamoyl chloride in 100 ml. of benzene. The resulting mixture is stirred at room temperature overnight, then poured into 100 ml. of water and acidified. The organic phase is extracted once with dilute aqueous acid. The combined aqueous phases are extracted twice with ether, then made basic to about pH 10 and extracted three times with chloroform. The combined chloroform extracts are dried over magnesium sulfate and the solvent is removed by evaporation. The residue is chromatographed, then distilled in vacuo to give 2-methoxy-N,N-dimethyl-2-(2-pyridyl)thioacetamide.

1. additionTo this mixture is added dropwise 10.0 g
2. additionpoured into 100 ml
3. extractionThe organic phase is extracted once with dilute aqueous acid
4. extractionThe combined aqueous phases are extracted twice with ether
5. extractionextracted three times with chloroform
6. dry with materialThe combined chloroform extracts are dried over magnesium sulfate
7. customthe solvent is removed by evaporation
8. customThe residue is chromatographed
9. distillationdistilled in vacuo