1-bromoacenaphthylene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: After the reaction solution was cooled, separated potassium bromide was removed by filtration, methanol was distilled, washed 3 times with water, and the benzene solution was concentrated and dropwise added into cold acetone (0°~-10° C.), to obtain reprecipitate of 140 g of condensed bromoacenaphthylene. Elemental analysis showed that the composition of the condensate corresponded to (C12H4.4 Br2.7)m and the yield from acenaphthene was 76.8%. After the reaction solution was cooled separated potassium bromide was removed by filtration, methanol was distilled washed 3 times with water the benzene solution was concentrated dropwise added into cold acetone (0°~-10° C.) to obtain

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1 mol of 1,2,3,5-tetrabromoacenaphthlene (C12H6Br4) in 500 g of benzene and 2 mols of potassium bromide and 0.2 mols of potassium bromate in 600 g of water was placed in a three-necked flask and stirred vigorously in a dark place. Two mols of concentrated sulfuric acid diluted with an equal volume of water was added dropwise to the mixture under agitation at about 10° C. Following a 3-hr reaction, the benzene layer was washed sequentially with water, aqueous caustic soda (2%) and water, and dried with silica gel. A solution of the dried benzene was transferred to a three-necked flask where it was dehydrobromated with a solution of about 2 mols of potassium hydroxide in hot ethanol that was added dropwise through the dropping funnel. After the reaction, the benzene layer was washed with water and dried. After distilling benzene off under vacuum, the residue was washed thoroughly with hot acetone and dried to provide a bromoacenaphthylene condensate. It was estimated by elemental analysis that the condensate had a rational formula of (C12H3.7 Br2.9)1. GPC showed that it had a degree of condensation l in the range of from 2 to 5. was placed in a three-necked flask was added dropwise to the mixture under agitation at about 10° C Following a 3-hr reaction the benzene layer was washed sequentially with water, aqueous caustic soda (2%) and water dried with silica gel A solution of the dried benzene was transferred to a three-necked flask was added dropwise through the dropping funnel After the reaction the benzene layer was washed with water dried After distilling benzene off under vacuum the residue was washed thoroughly with hot acetone dried

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: After the reaction solution was cooled, separated potassium bromide was removed by filtration, methanol was distilled, washed 3 times with water, and the benzene solution was concentrated and dropwise added into cold acetone (0°~-10° C.), to obtain reprecipitate of 140 g of condensed bromoacenaphthylene. Elemental analysis showed that the composition of the condensate corresponded to (C12H4.4 Br2.7)m and the yield from acenaphthene was 76.8%. After the reaction solution was cooled separated potassium bromide was removed by filtration, methanol was distilled washed 3 times with water the benzene solution was concentrated dropwise added into cold acetone (0°~-10° C.) to obtain