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【求助】以下物质的物性（颜色以及熔或沸点）
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求助以下物质的物性（颜色以及熔或沸点） [ Last edited by mooncakexzj on 2009-3-11 at 22:17 ] |
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mooncakexzj(金币+1,VIP+0):xiexie参与讨论 3-12 20:30
mooncakexzj(金币+1,VIP+0):xiexie参与讨论 3-12 20:30
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Chemosphere, 38(13), 3119-3130; 1999 环境科学, 8(2), 15-20; 1987 这两个文献里有这个物质，第一个是关于其合成的 2,4,6-trinitrobenzyl alcohol (11) The trinitrobenzyl alcohol was synthesized in a two-step reaction via trinitrobenzyl bromide. The synthesis was adapted from 13, 14. A solution of hypobromite was prepared by adding 5 mL of bromine to a chilled solution of 8.5 g of sodium hydroxide in 100 mL of water, stirring the solution until all the bromine had reacted and a clea, yellow solution formed, and then diluting to 150 mL with water. A solution of 5 g (0.02 mol) 2,4,6-trinitrotoluene in 100 mL of THF/methanol 1:1 (v/v) was chilled to -10 !aCin an ice-salt bath, then added at once, with rapid stirring, to 50 mL of the sodium hypobromite solution which was chilled to a slush. The temperature of the reaction mixture was kept below 5!aCduring 0.5 min of reaction time and then the bright red mixture was quenched in 500 mL of water containing 10 mL of concentrated hydrochloric acid. An oil separated after about 1 hour, the aqueous layer was decanted from the oil, and the product was washed with ice-water and then extracted with diethyl ether. The ether solution was dried over anhydrous magnesium sulfate and filtered, and the ether was removed by evaporation leaving an orange-yellow oily residue. Without further purification the residue was used for the second reaction step. 1 L of water was added and he solution boiled for 8 h under reflux. The solvent was evaporated and again an oily residue remained which was purified by column chromatography on silica gel (70-230 mesh) with ethyl acetate/petrol ether 1:3 v/v). The product was eluted in the fractions 400 -600 ml. ~H-NMR (300 MHz, CD3CN): 5 = 4.97 (s, 2 H), 8.79 (s, 2 H) [ Last edited by zwj6800 on 2009-3-12 at 20:27 ] |
2楼2009-03-12 20:26:43
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