Methyl iodide → HCID 21699015, compound

Participants

Reaction Steps

7-Methoxy-2-mercapto-4-oxo-4H-1-benzothiopyran (2.00 g, 8.92 mmol) was dissolved in DMF (15 ml) and gradually added with sodium hydride (505.8 mg, 11.59 mmol) over 30 minutes in the ice bath and under nitrogen atmosphere. After removal of the ice bath and stir for 12 hours, the solution was added with methyl iodide (0.83 ml, 13.37 mmol) and further stirred for 3 hours. The reaction liquid was injected into the cooled aqueous solution (100 ml) of saturated ammonium chloride. The precipitated crude crystals were filtrated and fully washed with water and dried in a desiccator under reduced pressure. The crude crystals were washed with the ether-hexane solution to obtain 1.77 g (yield: 83%) of 7-methoxy-2-methylthio-4-oxo-4H-1-benzothiopyran as light yellow powder.

Provenance & Evidence