ChemicalBook CAS DataBase List 2-Bromoanthracene

2-Bromoanthracene synthesis

8synthesis methods

Product Name:2-Bromoanthracene
CAS Number:7321-27-9
Molecular formula:C14H9Br
Molecular Weight:257.13

572-83-8 Synthesis

572-83-8
213 suppliers
$6.00/1g

7321-27-9
255 suppliers
$6.00/250mg

Yield:7321-27-9 82.02%

Reaction Conditions:

Stage #1: 2-bromoanthracene-9,10-dionewith potassium borohydrate;1-methoxy-2-(2-methoxyethoxy)ethane at 105; for 0.5 h;
Stage #2: with Aluminum Chloride at 30 - 110; for 0.333333 h;Concentration;Temperature;

Steps:

In a preferred embodiment,To a 500 mL three-necked flask was added 275.0 g diglyme,68.0 g (0.51 mol) of aluminum chloride solid was added slowly,The control temperature was 60 ° C,About 20min feeding is completed,The system becomes gray or milky white turbidity.Cooling to 30 ,stand-by.A further 1 L three-necked flask was charged with 49.2 g (0.17 mol) of 2-bromoanthraquinone,200.0 g diglyme,Stir,27.5 g (0.51 mol) of potassium borohydride was added,The system becomes yellow-green turbidity,Heating up to 105 ° C,And heat for 30 minutes,During the heating process, the system changed from yellow-green turbidity to pink turbidity,Finally into brown turbidity.Insulation is completed,The above-mentioned aluminum chloride solution was slowly added to the system,Control the internal temperature between 90 ~ 110 ,Drop before the first 1/3 of the exothermic reaction,After 2/3 of the process, the endothermic reaction,Dripping with the full range of bubbles,System from brown turbidity into bright yellow turbidity,Finally turned into yellow turbidity.The feeding process is about 20 minutes.Feeding is completed,Quickly cool the water bath to 40 ° C.The system was poured into concentrated hydrochloric acid / water / ethanol (100 g / 400 g / 300 g)System exotherm, accompanied by a large amount of gas generated.Hydrolysis process control system temperature below 60 .Hydrolysis is completed, cooling to 25 ,Filter,100.0g of water and 100.0g of anhydrous ethanol were leaching filter cake was yellow filter cake,This product is crude product.According to crude:Anhydrous ethanol = 1: 10 by the addition of absolute ethanol,Heating up to 50 ~ 60 ,Stirring for 1.0 hr,Cooling to 25 ~ 30 ,Insulation 0.5hr, suction filter,A small amount of anhydrous ethanol leaching filter cake was white solid,This is the product quality,Dried (50 ° C, 200 Pa, 5 hr) to give 35.8 g of a white powdery solid,This is the product quality, the yield of 82.02%

References:

CN106916049,2017,A Location in patent:Paragraph 0031; 0032; 0033; 0034; 0035; 0036; 0037-0042