EXPERIMENTAL PROCEDURE Assemble the reaction apparatus as shown in the picture,

Question

EXPERIMENTAL PROCEDURE Assemble the reaction apparatus as shown in the picture, make sure that all the joints are tightly connected. Attach the gas trap to contain the gaseous HCl formed during the reaction. All glassware must be completely dry before starting the r Aluminum chloride and acetyl chloride react vigorously with water. All mass measurements and transfer chemicals must avoid of contact with water and be performed in the fume hood. Glassware must be stopper as carrying back and forth between the fume hood and work bench Weigh 7.0 g of anhydrous aluminum chloride (AICI, in the fume hood and transfer it to a 100 mL 3-neck round bottom flask (RB). Add 12.5 mL of dichloromethane (CH2cL into the same flask and stopper it with a Teflon stopper immediately before transport it back to your bench in an ice water bath. Place a Assemble the reaction apparatus as shown in Figure 8. Cool the fl stir bar into the flask and begin stirring gently. Bring a 125 mL separatory funnel to the hood and transfer 4.0 gofacetyl chloride and 7.5 mL f CH2Clz into the separatory funnel using the ring provided in the fume hood to support the eparatory funnel. Attach this separatory funnel to the 3 neck reaction flask. slowly drip the acetyl hloride and CH2Cl2 mixture in the separatory funnel into the reaction flask over a period of 10 minutes. An exothermic reaction occurs when acetyl chloride is added. The solution should become uniformly yellow. If a cloudy off-white mixture is observed, it is likely that the reaction absorbed moisture and the catalyst was deactivated When the electrophile is activated (yellow color appeared), mix 0.0375 moles of toluene and 5.0 mL in the separatory funnel. Do not remove the separatory funnel from the reaction of CH2C12 the the top of the separatory funnel to flask, just close the stopcock and remove drying tube from add the reagents. Slowly add the solution into the RB flask drop wise o a period of 10 minutes At this point the solution should turn amber in col After the addition of all reagents is complete, remove the ice bath and let the mixture come to room temperature. Stir the reaction mixture for an additional 15 minu

Explanation / Answer

After stirring for an additional 15 minutes at room temperature, the reaction
mixture can be pour carefully and slowly, with stirring, into about 25 g of ice and 15 mL of
concentrated HCl in a beaker. Then transfer the mixture to a separatory funnel and collect the organic layer. Extract The aqueous layer with 20 mL of methylene chloride.
The combined organic layers extract with two portions of saturated sodium bicarbonate
and dried over anhydrous MgSO4. The drying agent can be remove by gravity filtration into an
appropriately sized round-bottomed flask. The methylene chloride can be remove by rotary
evaporation. If necessary, a flask
can be set up for simple distillation and insulated with aluminum foil or glass wool. The mixture
was distilled, raising the setting on the variac as necessary. If residual starting material was
present, it distilled around 150o
C, while each of the products has a boiling point greater than
200o
C.

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