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19 Nov 2019
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Organic Chemistry Laboratory II EXPERIMENTAL PROCEDURE . Borrow a stir bar from the instructor 2. Place 3.3 g of acetanilide into a 125-mL Erlenmeyer flask and then add 5 is of p-Nitroacetanilide mL of glacial (concentrated) acetic acid (CAUTION: strong irritant). Warm the flask on a hot plate in the hood until the acetanilide dissolves. Cool the flask in an ice bath to about 20°C; then add 5 mL of cold, concentrated sulfuric acid. The temperature of the mixture will rise to about 60°C. Chill the solution to about 10°C in an ice bath. (The solution may become very viscous.) 3. Mix 1.8 mL of concentrated nitric acid and 2.5 mL of concentrated sulfuric acid in a 50-mL Erlenmeyer flask (CAUTION: Use extreme care when preparing this nitrating mixture), and chill the flask in an ice bath for~4 minutes 4. When both solutions are cold, slowly add the nitrating mixture, 1 mL at a time, to the constantly stirred acetanilide solution. Keep the reaction flask in an ice bath so that the temperature of the reaction mixture is maintained between 10 - 20°C. The entire addition requires about 15 minutes. 5. After the addition is completed, allow the reaction to proceed at room temperature for 30 minutes (keep the stirrer going). Monitor the temperature; if it rises above 30°C, chill the flask in an ice bath to just below 30°C. Should the re-chilling be necessary, allow the reaction to proceed for an additional 10 minutes. 6. Pour the reaction mixture into a 250-mL beaker containing 50 mL of water and about 15 g of cracked ice. Stir the mixture for a minute or so during this time a light yellow solid should form. [If a white solid forms, then you have recovered unreacted acetanilide. If a dark yellow or yellow-orange solid is recovered, then the product has undergone hydrolysis. Should any of these two things occur, you must start the reaction all over again - consult with your instructor if you are unsure about the color.] 7. Vacuum filter the solution. Press down on the light yellow solid with a clean 50 mL beaker or Erlenmeyer flask to remove as much of the aqueous solution as possible. (CAUTION: Nitro compounds are toxic and can be absorbed through the skin.)
This is the only info I get
Organic Chemistry Laboratory II EXPERIMENTAL PROCEDURE . Borrow a stir bar from the instructor 2. Place 3.3 g of acetanilide into a 125-mL Erlenmeyer flask and then add 5 is of p-Nitroacetanilide mL of glacial (concentrated) acetic acid (CAUTION: strong irritant). Warm the flask on a hot plate in the hood until the acetanilide dissolves. Cool the flask in an ice bath to about 20°C; then add 5 mL of cold, concentrated sulfuric acid. The temperature of the mixture will rise to about 60°C. Chill the solution to about 10°C in an ice bath. (The solution may become very viscous.) 3. Mix 1.8 mL of concentrated nitric acid and 2.5 mL of concentrated sulfuric acid in a 50-mL Erlenmeyer flask (CAUTION: Use extreme care when preparing this nitrating mixture), and chill the flask in an ice bath for~4 minutes 4. When both solutions are cold, slowly add the nitrating mixture, 1 mL at a time, to the constantly stirred acetanilide solution. Keep the reaction flask in an ice bath so that the temperature of the reaction mixture is maintained between 10 - 20°C. The entire addition requires about 15 minutes. 5. After the addition is completed, allow the reaction to proceed at room temperature for 30 minutes (keep the stirrer going). Monitor the temperature; if it rises above 30°C, chill the flask in an ice bath to just below 30°C. Should the re-chilling be necessary, allow the reaction to proceed for an additional 10 minutes. 6. Pour the reaction mixture into a 250-mL beaker containing 50 mL of water and about 15 g of cracked ice. Stir the mixture for a minute or so during this time a light yellow solid should form. [If a white solid forms, then you have recovered unreacted acetanilide. If a dark yellow or yellow-orange solid is recovered, then the product has undergone hydrolysis. Should any of these two things occur, you must start the reaction all over again - consult with your instructor if you are unsure about the color.] 7. Vacuum filter the solution. Press down on the light yellow solid with a clean 50 mL beaker or Erlenmeyer flask to remove as much of the aqueous solution as possible. (CAUTION: Nitro compounds are toxic and can be absorbed through the skin.)
Lelia LubowitzLv2
20 May 2019