Question

PROCEDURE CAUTION!!! Nitric acid and sulfuric acid are strong and corrosive acids. For that reason, avoid inhaling its vapors or causing any contact with the skin or clothing. Wear your protective glasses at all times. Use the extractors to work with these acids. A. Nitration of methyl benzoate 1. Preparation of the reactants. In the extractor you will find a burette with concentrated sulfuric acid, a second burette with concentrated nitric acid, clearly identified. Familiarize yourself with the scales of both burettes to be able to measure the volume of the acids correctly. Then, transfer to a large, clean, dry test tube labeled "A" 1.0 mL of concentrated sulfuric acid (H2SO4), introduce the thermometer (do not remove it from the test tube until the end of the experiment) and cool its contents to 0 °C, placing the test tube with a 3-fingered clamp in an ice/water bath. Add from the third burette 0.50 mL of methyl benzoate to test tube "A" that is at temperature of 0 °C. Then, remove the test tube from the ice/water bath and let the temperature of the test tube reach about 20 °C, slightly shaking the contents of the tube with the thermometer. Re-cool the test tube until its contents again indicate the temperature of 0 °C. While cooling the test tube "A", prepare another test tube (medium or small size), clean and dry, labeled "MN" (nitrating mixture). In the extractor, carefully transfer to the "MN" test tube first 0.4 mL of concentrated nitric acid (HNO3) and then 0.4 mL of concentrated sulfuric acid. Shake the warm mixture carefully with a clean, dry glass rod. 2. Nitration With a clean, dry Pasteur-type dropper, transfer slowly (this is the crucial part of the experiment and dropwise the nitrating mixture from the "MN" test tube to the test tube "A" containing the acidified methyl benzoate found in the ice/water bath , but in such a way that the temperature stays between 10 and 15 ° C. If the reaction temperature is lower, the reaction is very slow and if it is higher than 15 °C, a greater amount of secondary products could be formed, which can be controlled by maintaining the temperature in the indicated range by means of a slow addition

Answer 1

& Fins According to the data given by you: Molecular (C&H ₂ O 2 HNO₂ 63.01% 98.079 149,15 loomua 136.15 . Quontity (g) 0.54 1.H2 504 CzH7NO4 mass (almoly 3.97X1077.52X1311.2 X10 2710-2 12 Volcarra on ois out 1519 Density gland 1,094 13 Physiel BP-23°C MP-10°C content [1] 0.84 0.409 1.23 Mo 11.83 1.20

givenas. :- OCH 20 HNO, would be the line 149. 15 of m-nitro- The reaction which takes place a OCH, +HNO3 + H₂SO4 → From the above data, we conclude that benzoate 0 409 9 of HNO, wille produe m-nitrobenzoate. 0,409 X 149,15 63.00

09 oo - We use the process of recrystallization for purification of methyl m-nitrobenzoate 10 which is extracted out itself after purif Ladvent used for purification is thara ication of methyl m-nitroberseite - Weight of pure product a given to as 12 0.849 Percentage yield of pure product theoretical gield of fire product 0.84 Xido = 86. sgy cu 13 Xroo 15 N O. 9