2-(4-(溴甲基)苯基)乙酸乙酯

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 25.7 g of ethyl 4-bromomethylphenylacetate and 28 g of hexamethylenetetramine are dissolved in 200 ml of 20% acetic acid, heated to 100° C. with stirring and stirred for four hours. The reaction solution is allowed to cool and sufficient sodium carbonate is added until a saturated solution is obtained. This solution is extracted with ether, dried and the ether is then removed. The residue is purified by chromatography (silica gel/methyl t-butyl ether/ether 1:1). stirred for four hours to cool is obtained This solution is extracted with ether dried the ether is then removed The residue is purified by chromatography (silica gel/methyl t-butyl ether/ether 1:1)

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

实验步骤: 1.00 g of 2-[4-(bromomethyl)phenyl]acetic acid was suspended in 5 mL of a 4M solution of hydrogen chloride in ethanol, and this suspension was stirred for 2 hours at room temperature. The reaction mixture was concentrated under reduced pressure to yield 0.954 g of ethyl 2-[4-(bromomethyl)phenyl]acetate as light brown oil. The reaction mixture was concentrated under reduced pressure

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 25.7 g of ethyl 4-bromomethylphenylacetate and 28 g of hexamethylenetetramine are dissolved in 200 ml of 20% acetic acid, heated to 100° C. with stirring and stirred for four hours. The reaction solution is allowed to cool and sufficient sodium carbonate is added until a saturated solution is obtained. This solution is extracted with ether, dried and the ether is then removed. The residue is purified by chromatography (silica gel/methyl t-butyl ether/ether 1:1). stirred for four hours to cool is obtained This solution is extracted with ether dried the ether is then removed The residue is purified by chromatography (silica gel/methyl t-butyl ether/ether 1:1)

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

实验步骤: To a solution of 3-[3-phenyl-8-(trifluoromethyl)quinolin-4-yl]phenol (0.178 g, 0.487 mmol), and potassium carbonate (0.134 g, 0.974 mmol), in DMF at 120° C. is added 4-bromomethylphenylacetic acid ethyl ester (0.334 g, 1.46 mmol), drop wise over 2 h. After an additional 2 h, the cooled reaction is poured into 2N aq HCl and extracted with ethyl acetate. The combined extracts are washed with sat aq NaHCO3, water, brine, and dried with magnesium sulfate. The extracts are concentrated and the residue is chromatographed with 1:9 ethyl acetate:hexanes to afford the title compound as a syrup (0.051 g, 37%). MS m/z 542; HRMS: calcd for C33H26NF3O3+H, 542.19430; found (ESI, [M+H]+), 542.194. After an additional 2 h the cooled reaction extracted with ethyl acetate The combined extracts are washed with sat aq NaHCO3, water, brine dried with magnesium sulfate The extracts are concentrated the residue is chromatographed with 1:9 ethyl acetate

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

实验步骤: 1.00 g of 2-[4-(bromomethyl)phenyl]acetic acid was suspended in 5 mL of a 4M solution of hydrogen chloride in ethanol, and this suspension was stirred for 2 hours at room temperature. The reaction mixture was concentrated under reduced pressure to yield 0.954 g of ethyl 2-[4-(bromomethyl)phenyl]acetate as light brown oil. The reaction mixture was concentrated under reduced pressure

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 25.7 g of ethyl 4-bromomethylphenylacetate and 28 g of hexamethylenetetramine are dissolved in 200 ml of 20% acetic acid, heated to 100° C. with stirring and stirred for four hours. The reaction solution is allowed to cool and sufficient sodium carbonate is added until a saturated solution is obtained. This solution is extracted with ether, dried and the ether is then removed. The residue is purified by chromatography (silica gel/methyl t-butyl ether/ether 1:1). stirred for four hours to cool is obtained This solution is extracted with ether dried the ether is then removed The residue is purified by chromatography (silica gel/methyl t-butyl ether/ether 1:1)