叔戊基苯

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: 74 g (0.5 mole) of phthalic anhydride were reacted with 128 g (1.05 moles) of AlCl3 and 25 g (0.2 mole) of diethylzinc in 74 g of tert-amylbenzene, similarly to Example 1. After the mixture had been worked up, 118 g (80% of theory) of pure 2-(4'-tert-amylbenzoyl)-benzoic acid were obtained.

反应条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 600 ml autoclave equipped with a magnetic stirrer, Solid Base A (0.45 g) and cumene (240 g) were charged under nitrogen, heated to 160° C. while stirring at 1,000 rpm and then reacted at the same temperature for 3 hours while supplying ethylene gas under pressure of 10 kg/cm2G. to produce tert.-amylbenzene (hereinafter referred to as "TAB"). In a 600 ml autoclave equipped with a magnetic stirrer reacted at the same temperature for 3 hours

反应条件: temp:105.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 600 ml autoclave equipped with a magnetic stirrer, Solid Base A (0.39 g) and cumene (240 g) were charged under nitrogen, heated to 105° C. while stirring and then reacted at the same temperature for 1.5 hours while supplying ethylene gas under pressure of 10 kg/cm2G. to produce tert.-amylbenzene (hereinafter referred to as "TAB"). In a 600 ml autoclave equipped with a magnetic stirrer reacted at the same temperature for 1.5 hours

反应条件: temp:35.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A glass reactor equipped with a mechanically driven stirrer, addition funnel and hydrogen bromide trap was charged with 300 g (2.02 mole) of t-amylbenzene and 8 g of iron filings. Bromine (374 g, 2.02 mole) was added dropwise at a rate such that the temperature of the reaction mixture was maintained at about 35° C. The reaction mixture was stirred for 15 hours while being heated to a temperature of 50° C. The contents of the reactor were then cooled and combined with 200 cc of a saturated aqueous sodium bisulfite solution. After being stirred for a few moments the reaction mixture was filtered. The organic layer was then separated and combined with a quantity of anhydrous magnesium sulfate to remove any water present. The liquid phase was then separated and distilled under a pressure of 0.1 mm of mercury. The fraction boiling from 70° to 75° C. was collected and analyzed for carbon, hydrogen and bromine. while being heated to a temperature of 50° C The contents of the reactor were then cooled After being stirred for a few moments the reaction mixture was filtered The organic layer was then separated to remove any water present The liquid phase was then separated distilled under a pressure of 0.1 mm of mercury boiling from 70° to 75° C. was collected

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

实验步骤: 74 g (0.5 mole) of phthalic anhydride were reacted with 128 g (1.05 moles) of AlCl3 and 25 g (0.2 mole) of diethylzinc in 74 g of tert-amylbenzene, similarly to Example 1. After the mixture had been worked up, 118 g (80% of theory) of pure 2-(4'-tert-amylbenzoyl)-benzoic acid were obtained.

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

实验步骤: 74 g (0.5 mole) of phthalic anhydride were reacted with 128 g (1.05 moles) of AlCl3 and 25 g (0.2 mole) of diethylzinc in 74 g of tert-amylbenzene, similarly to Example 1. After the mixture had been worked up, 118 g (80% of theory) of pure 2-(4'-tert-amylbenzoyl)-benzoic acid were obtained.

反应条件: temp:0.00; pressure:0.00; stir:

实验步骤: 投料: 三口瓶中加入三氯化铝（33.7.0g，1.5eq）和超干DCM（300ml），在冰浴下降温至0℃-5℃，再加入丙酰氯（18.7g，1.2eq），保持温度搅拌15min，再将SM1（25g,1.0eq）缓慢滴加至反应液中，控制温度不超过5℃，滴加完毕保持温度搅拌1h。 13：30 送样LCMS监测反应进程不出产物MS，点板TLC（PE:EA=10:1)产物极性比原料大，反应体系未见原料，降温加水淬灭，缓慢滴加比较剧烈并且有白色固体析出，用甲醇溶解点板TLC仅有微量产物，剩余体系用DCM萃取三次，合并有机相干燥浓缩，黄色油状（28g）直接用于下一步。

实验步骤: 02-12 09:22: 取50ml单口瓶，加入C4X-154210-SM1（0.15g 1eq）和DCM（4ml），室温下分批加入二溴海因（0.58g 2eq），反应液室温搅拌过夜。 GCMS监测（154210-s1-br2-n），无反应

实验步骤: 投料: 取50ml单口瓶，加入C4X-154210-SM1（0.15g 1eq）和DCM（4ml），室温下分批加入NBS（0.27g 1.52eq），反应液低温反应仪-3℃中搅拌过夜。 GCMS监测（154210-s1-n），无反应

实验步骤: 投料: 取100ml单口瓶，加入碘（2.2g 0.64eq）、高碘酸钠（0.62g 0.21eq）醋酸（9.3ml 12eq）、醋酸酐（9.3ml）和硫酸（1.55ml 2.14eq），最后加入M-C4X-154248-SM1（2g 1eq），添加完毕后，反应液室温下搅拌过夜 GCMS（154248-s1-n），原料剩余50%，有产物ms生成 后处理：反应液用硫代硫酸钠溶液进行淬灭，由棕褐色溶液转变为黄色溶液，加入石油醚和水进行萃取，取有机相，水相经确认，无产物，将有机相浓缩重投 重复上述投料操作 GCMS（154248-s1-n），原料反应完全，有产物ms生成 后处理：反应液经硫代硫酸钠溶液淬灭，加入石油醚和水萃取，取有机相并用无水硫酸钠干燥，抽滤，得淡黄色油状物 纯化：粗品经硅胶柱层析分离纯化（PE=100%，300-400目硅胶）,无干净层析液 粗品经自动过柱机分离纯化（ACN：H2O=90:10，3g样，用10ml乙腈溶解，120g反相柱进样1.5-2ml，进样浓度高则分离度差，60%乙腈梯度开始过），得淡黄色油状物1.5g。