实验二十三 对溴苯胺的合成及结构表征(~25学时)(Experiment twenty-three synthesis and structure characterization of aniline bromide (~25 hours)).docVIP
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实验二十三 对溴苯胺的合成及结构表征(~25学时)(Experiment twenty-three synthesis and structure characterization of aniline bromide (~25 hours))
实验二十三 对溴苯胺的合成及结构表征(~25学时)(Experiment twenty-three synthesis and structure characterization of aniline bromide (~25 hours))
Experiment twenty-three synthesis and structure characterization of aniline bromide (~25 hours)
Experimental purpose
1. to understand the specific reaction of the special bromine reagent 2,4,4,6- four bromo -2,5- cyclohexene -1- ketone to aromatic amines.
2. strengthen the recrystallization and vacuum distillation and other experimental skills.
3. to study the purity of the identified products by tlc.
4. the structure of the product was characterized by IR and nuclear magnetic resonance spectroscopy.
Two 、 experimental principle
One
EMBED ChemWindow.Document
Two
EMBED ChemWindow.Document
Three
EMBED ChemWindow.Document
Three 、 main instruments and reagents
Grinding glass instrument, electromagnetic stirrer, rotary evaporator, high vacuum oil pump
Phenol and aniline bromine hydrated sodium acetate acetic acid sodium hydroxide dichloromethane petroleum ether hydrochloride
Four, experimental steps
1. preparation of tribromophenol
Take 3.4 grams (0.036mol) of phenol in 250 ml three flasks, add 100ml water, mix with electromagnetic stirring, and the flask is equipped with a drip funnel, a condensing tube and a gas absorption device. 17.2 grams (0.108mol) through [1] into the dropping funnel, covered with water 20ml. Add bromine [2] at room temperature stirring, and precipitate white precipitate immediately in the reaction. After adding bromine, the reaction mixture was stirred at room temperature to half an hour, and then filtered, the white solid product. The product is weighed after airing, about 11.4 grams (96%), Mp = 93-95oC.
Preparation of 2.2,4,4,6- four bromo -2,5- cyclohexene -1- ketone
11.2 grams (0.034mol) tribromophenol, 4.6 grams (0.034mol) sodium acetate hydrate (CH3COONa. 3H2O)
Added to 80ml glacial acetic acid in turn. Stirring, slowly heating to mixed solution temperature of about 70oC, until the solid completely dissolved, cool down
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