Triobenzenetricarboxylic Acid Synthesis Lab Report
TITLE OF THE PROJECT : Synthesis and Characterisation of Benzenetricarboxylic (BTC) linkers.
Introduction :
In this semester, my project is on 1,3,5-benzenetricarboxylic acid (BTC) i.e ; Synthesis and preparation of methoxy-1,3,5-benzenetricarboxylic acid , brown-BTC, nitro-BTC and acetamide –BTC.
What is BTC ? Trimesic acid ,which is also known as 1,3,5-tricarboxylic acid. It is a benzene derivative with three carboxylic acid groups. Trimesic acid is a planar molecule .It is one of the four benzenecarboxylic acids with this property. Trimesic acid can be combined with para-hydroxypyridine to make a water-based gel, which will be stable up to 95 °C. Trimesic acid crystallizes from water in a hydrogen bonded hydrated network with wide
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It has a chemical formula as C_9 H_6 O_6. It is stable at normal conditions a,but may be light sensitive. It is off-white powder. It is classified as Carbocyclic Carboxylic acids.
Trimesic acid Trimesic acid - 3D Ball structure
Preparation of methoxy-1,3,5-benzenetricarboxylic acid : Firstly take DMF , 2,6-bis(hydroxymethyl)-p-cresol, K_2 CO_3 and CH_3I . Now add 2,6-bis(hydroxymethyl)-p-cresol, k_2 〖CO〗_3 and 〖CH〗_3I in a 100ml beaker and put it aside Now slowly add DMF into that above mixture and keep it in a stirrer for 3 days. After 3 days we can find a yellow milky solid in that round bottled flask Dilute it in water and extract the ethylacetate
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Take 20g of 2-bromomesitylene and add it to 5g NaOH in a 250ml aqueous solution Now add potassium permanganate in many batches for 2 hrs to the solution Stirr it continuously with out any heating After 2 hrs heat it @95^oc and stirr it continuously for 3 days A Brown slurry is formed after 3 days, from this we can extract large amount of MnO_2 by filtering Also we can extract aqueous solution with ethyl ether continuously Remove ethyl ether in vacuum so that we can yield the product bromo-BTC
Mesitylene Bromide 1H
Mesitylene Bromide 13C Bromo-BTC 1H Bromo-BTC 13C
Preparation of nitro-1,3,5-benzenetricarboxylic acid :
Firstly take 2-nitromesitylene ,NaOH, and potassium permanganate .put them aside Now , take 20g of 2-nitromesitylene and add it to 5g NaOH in an aqueous solution 250ml Take 85g of potassium permanganate and add it to the solution for 2 hrs through droplets. Stirr it continuously without any
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