4-异丁基苯乙酮

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: A solution of 4-isobutylacetophenone (2.0 g), 3-benzyl-3H-imidazole-4-carbaldehyde (2.1 g) and 48% sodium hydroxide (0.65 ml) in methanol (20 ml) is heated at 55-60° C. for 6 hours. The reaction mixture is then cooled in an ice bath. The resulting precipitate is filtered, and rinsed with methanol. The yield is 2.5 g. The reaction mixture is then cooled in an ice bath The resulting precipitate is filtered rinsed with methanol

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

实验步骤: Isobutylbenzene (IBB) (10.2 lb/hr) and a solution of HF containing 13 wt % HOAc and 12 wt % acetyl fluoride (AcF) (153 lb/hr) were fed into reactor 1 through line 4. The mixture was reacted at 60° C. for 1.5 hrs to produce the desired 4-isobutylacetophenone product. were fed into reactor The mixture was reacted at 60° C. for 1.5 hrs

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

实验步骤: Isobutylbenzene (IBB) (10.2 lb/hr) and a solution of HF containing 13 wt % HOAc and 12 wt % acetyl fluoride (AcF) (153 lb/hr) were fed into reactor 1 through line 4. The mixture was reacted at 60° C. for 1.5 hrs to produce the desired 4-isobutylacetophenone product. were fed into reactor The mixture was reacted at 60° C. for 1.5 hrs

反应条件: temp:5.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Bromine (1.25 ml; 25 mmol) is added dropwise to a solution of 4′-isobutylacetophenone (3.52 g; 20 mmol) in 60 ml of ethanol cooled down to approximately 5° C. After stirring the reaction mixture for 30 minutes at this temperature, stirring is continued for one hour at ambient temperature. The reaction medium, to which small portions of toluene are added, is concentrated to dryness. After purification on a silica column (eluent: ethyl-heptane acetate: 5-95), a colourless oil is obtained with a yield of 57%. stirring is continued for one hour at ambient temperature is concentrated to dryness After purification on a silica column (eluent: ethyl-heptane acetate: 5-95) a colourless oil is obtained with a yield of 57%

反应条件: temp:5.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Bromine (1.25 ml; 25 mmol) is added dropwise to a solution of 4′-isobutylacetophenone (3.52 g; 20 mmol) in 60 ml of ethanol cooled down to approximately 5° C. After stirring the reaction mixture for 30 minutes at this temperature, stirring is continued for one hour at ambient temperature. The reaction medium, to which small portions of toluene are added, is concentrated to dryness. After purification on a silica column (eluent: ethyl-heptane acetate: 5-95), a colourless oil is obtained with a yield of 57%. stirring is continued for one hour at ambient temperature is concentrated to dryness After purification on a silica column (eluent: ethyl-heptane acetate: 5-95) a colourless oil is obtained with a yield of 57%

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

实验步骤: 24.8 g (0.2 mole) of thioanisole was heated to 90° C. with stirring, 27.8 g (0.22 mole) of dimethyl sulfate was added thereto at 90°-95° C. over a period of 30 minutes and stirred for another 30 minutes at the same temperature. To the reaction mixture, 100 ml of toluene was added portionwise so as to maintain the temperature above 80° C. and then the mixture was cooled gradually with stirring to afford a suspension of phenyldimethylsulfonium methylsulfate in quantititative yield. To the suspension, 26.4 g (0.15 mole) of p-isobutylacetophenone and 16.0 g (0.4 mole) of powdered sodium hydroxide was added and the mixture was stirred for 8 hours at 50° C. The reaction mixture was worked up in the same manner as described in Example 6 to afford 24.7 g of 2-(4-isobutylphenyl)-1,2-epoxypropane in 86.7% yield. stirred for another 30 minutes at the same temperature to maintain the temperature above 80° C. the mixture was cooled gradually with stirring to afford the mixture was stirred for 8 hours at 50° C

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

实验步骤: A solution of 4-isobutylacetophenone (2.0 g), 3-benzyl-3H-imidazole-4-carbaldehyde (2.1 g) and 48% sodium hydroxide (0.65 ml) in methanol (20 ml) is heated at 55-60° C. for 6 hours. The reaction mixture is then cooled in an ice bath. The resulting precipitate is filtered, and rinsed with methanol. The yield is 2.5 g. The reaction mixture is then cooled in an ice bath The resulting precipitate is filtered rinsed with methanol

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

实验步骤: A solution of 4-isobutylacetophenone (2.0 g), 3-benzyl-3H-imidazole-4-carbaldehyde (2.1 g) and 48% sodium hydroxide (0.65 ml) in methanol (20 ml) is heated at 55-60° C. for 6 hours. The reaction mixture is then cooled in an ice bath. The resulting precipitate is filtered, and rinsed with methanol. The yield is 2.5 g. The reaction mixture is then cooled in an ice bath The resulting precipitate is filtered rinsed with methanol

反应条件: temp:0.00; pressure:0.00; stir:

实验步骤: 投料: B6P89 平行反应瓶中加入加入0.88ml 4-异丁基苯乙酮（5mmol，1.0eq.，ρ=0.988）和2.5ml 95% 乙醇（0.2M），无色澄明，-30℃滴加0.73ml 氯化亚砜（10mmol，2.0eq.，ρ=1.64），溶液变亮黄色澄明。 保持低温反应。 \n监测: 溶液橙黄色，外温-5℃，反应液取样，加饱和碳酸氢钠溶液淬灭，加DCM萃取，DCM相TLC（PE:EA=30:1），原料点太浓，不确定反应情况。 180.30 鲜红色，反应液取样，加饱和碳酸氢钠溶液淬灭，加DCM萃取，DCM相TLC（PE:EA=30:1），仍有较多原料，有比原料极性小的新点。-20℃放置。 2/12 反应液取样，加饱和碳酸氢钠溶液淬灭，加DCM萃取，DCM相TLC（PE:EA=30:1），反应体系略杂，但仍有较多原料。\n后处理: 加水加DCM萃取，有机相点板有五个点，旋干过正相纯化。\n纯化: 正相纯化，PE:EA=30:1，除P1为黄色油状物外，其余点均为少量无色油状物。 2/13 P2取样加DMSO送HNMR（C4X-10828-1-1-P2），核磁谱图基线不平且很多杂峰，取样加CDCL3送HNMR（C4X-10828-1-1-P2-CDCL3）结构不对应。 2/14 P1、P3、P4取样加CDCL3送HNMR（C4X-10828-1-1-P1/3/4）结构均不对应。 视反应失败，重投，反应2小时即处理，不管原料是否消耗完。

实验步骤: 投料: B6P181 100ml单口瓶中加入7.7ml 4-异丁基苯乙酮（43.7mmol，1.0eq.，ρ=0.988）和20ml 95% 乙醇（~0.2M），无色澄明，冰盐浴-5℃搅拌5min后，滴加6.4ml 氯化亚砜（87.4mmol，2.0eq.，ρ=1.64），大量烟雾，溶液迅速变深黄色，最终为红褐色澄明。 N2置换，保持低温（-5~5℃）反应。\n监测: 反应液取样，加饱和碳酸氢钠溶液淬灭，加EA萃取，EA相TLC（PE:EA=30:1），余有较多原料，监测至14.00原料和产物1:1停止反应。\n后处理: 反应液加饱和碳酸氢钠溶液淬灭（有气泡，冰浴缓慢加），加EA萃取，有机相合并之前杂瓶旋干得黄色油状物约12g。\n纯化: 过硅胶柱纯化（PE:EA=50:1），纯化得纯瓶约1g，杂瓶约10g，重新过柱仍与原料点一起出，回收9.5g黄色油状物，直接投下一步。