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Chemistry Anailide

Essay by   •  April 13, 2011  •  Essay  •  867 Words (4 Pages)  •  1,873 Views

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The first step was the acetlation of aniline. 4.0ml of aniline was dissolved in 10 ml of acetic acid in a 100ml round bottomed flask. 5 ml of acetic anhyhydride was then added to the soultion and was mixed well by swirling. Care was taken when handling the flas as it was exothermic and became warm. Two boiling chips were then added to the flask and it was attached to the condensing column. The hoses for the water colling were then attached. They were added so water went in at the bottom and came out at the top. A gentle reflux was then heated for 15 minuts. After the 15 minutes the iron ring under the heating mantle was lowered and the flask was cooled slightly. 5mls of cold water was added cautiously through the top of the condnser into the reaction mixture. The solution was then boiled for an additional five minutes. This was done to hydrolize the unreacted acetic anhydride. After the mixture was boiled for five minutes, the reactin was cooled and then it was poured slowly with stirring into 30 ml of icew cold water. The mixture was allowed to stand for 15 minutes and stirred occasionally. The precipitate was then collected by suction filterartion using the Buchner funnel. The solid crystals were then washed with 10ml of cold water and replaced in the vacumm to dry them again. They were then left to dry untill the following week. The following week t, firstly 0.5g of the product was taken out and recrysttalised form about 15mls of water. This was done by 0.5g of the product being placed into an Erlenmeyer and 10 mls of water was added. A stirring rod was then used to dispeperse the the coumpund as much as possible. the supsnsion was then heated using the Bunsen burner. While the water was boiling the solution was stirred and more water was added until the material was dissolved. When the solution became clear it was removed from the heat and allowed to cool slowly at room tempearture and then it was put back in the water bath. The crystals were then collected by suction filteration using a hirsh funnel. The crystals were then left to dry. Then the niteronium ion was formed by dehydration of the nitric acid. The second step was the nitarion of acetanilide. Firstly 3.4g of the acetanilide was dissolved in 4ml of glacial acetic acid in a 125ml Erlenmeyer flask. The soultion was warmed slightly to get all the sold material to dissolev. When the solution was dissolved it was cooled in the ice bath. Crystals began to form. Then 5ml of concentrated ice cold sulphuric acid was was added slowly 1 ml at a time. This was done using a dropper. It was then left to cool in the ice bath until it reached 5 degreed Celsius. A nitrating mixture was then prepared in a separate Erlenmeyer flask. This was done by 1.8ml of concentrated bitric acid being added to 2,5ml of ice cold sulphuric acid. This was done in an ice bath and care ws taken as it was an exothermic reaction. The nitric acid was added very slowly using a dropper and then the nitrating mixture was

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