In a test tube, 0.514 g mercury was dissolved in 0.7 ml 90% nitric acid.
Then, 4.960 g of the product from Step 1 was dissolved in a flask with 25 ml methanol. 17.053 g zinc powder, the mercuric nitrate solution, and a
magnetic stir bar were added to the flask, which was fitted with a reflux condenser and an addition funnel containing 45 ml 12M hydrochloric acid. The
flask was heated to reflux, and then 10 ml of the acid were added quickly. The rest of the acid was added slowly over 3 hours, with vigorous magnetic
stirring.
Over this time, all of the zinc dissolved, and the mercury was reduced back to metallic form. When the reaction mixture had cooled, it was decanted
from the mercury, and 10M sodium hydroxide solution was added until it was basic to litmus paper (pH ~9). A white precipitate of zinc hydroxide
formed. The precipitate was filtered out, and the solution was extracted with 3 10 ml portions of toluene. Then, the toluene solution was extracted
with 3 5 ml portions of 3M hydrochloric acid. The acid was evaporated under vacuum to give 1.658 g white powder. The powder was recrystallized from
isopropanol to give 1.194 g colorless crystals. |
