2-甲基丁酰氯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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: To a suspension of AlCl3 (35.4 g) in CHCl3 (500 mL) at -10° C. was added dropwise 2-methylbutyryl chloride (31.3 g) followed by thioanisole (31.2 mL). The mixture was then stirred at r.t. for 20 min. and was then cooled back to 0° C. Water (200 mL) was then added over 30 min. The CHCl3 layer was separated and dried over MgSO4. After filtration and removal of the solvent, the residue was dried under vacuum at 80° C. for 2 h to give 35 g of the title compound. was then cooled back to 0° C The CHCl3 layer was separated dried over MgSO4 After filtration and removal of the solvent the residue was dried under vacuum at 80° C. for 2 h

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

实验步骤: A 500 mL RBF equipped with a mechanical stirrer was charged with AlCl3 (35.4 g) and CHCl3 (300 mL) and cooled in an ice bath. Then 2-methylbutanoyl chloride (31.4 g) was added over 0.5 h to the ice-cold suspension. Keeping the internal temperature <10° C., thioanisole (31.2 mL) was added dropwise over 1 h. After completion of addition, the resulting mixture was stirred at r.t. for 2 h. The resulting suspension was poured onto an ice-water mixture and stirred until decoloraton. The organic layer was separated, washed with water, dried over Na2SO4 and concentrated to dryness. The resulting white solid was swished in hexane and collected by filtration to give the title compound as a white solid. 1H NMR(CD3COCD3): δ0.88 (3H, t), 1.12 (3H, d), 1.47 (1H, m), 1.78 (1H, m), 2.57 (3H, s), 3.49 (1H, m), 7.37 (2H, d), 7.93 (2H, d). A 500 mL RBF equipped with a mechanical stirrer cooled in an ice bath was added dropwise over 1 h After completion of addition stirred until decoloraton The organic layer was separated washed with water dried over Na2SO4 concentrated to dryness collected by filtration

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 0.15 mole(15.0 g) of (S)-(+)-2-methylbutyric acid and 0.3 mole(35.5 g) of thionyl chloride in 100 ml of chloroform was refluxed for three hours. After chloroform and the excessive thionyl chloride had been distilled out at reduced pressure, the reaction solution was concentrated at reduced pressure to obtain 12.8 g of 2-methylbutyryl chloride. A suspension of 0.1 mole(13.3 g) of aluminium chloride in 100 ml of dry methylene chloride was cooled to 0° C., then 12.8 g of 2-methylbutyryl chloride was added dropwise thereto, and stirred for 30 min. Maintaining the mixed solution at 0° C., a solution of 0.08 mole(14.7 g) of 4-methoxybiphenyl in 80 ml of dry methylene chloride was added dropwise, and stirred for 10 hours at room temperature. The reaction mixture was decomposed by adding into ice and dil. hydrochloric acid, and the organic layer was washed with dil. hydrochloric acid and an aquious sodium hydrogen carbonate solution, and then dried with magnesium sulfate. The concentrated product was purified by column chromatography to obtain 10.3 g of 4'-methoxy-4-(2-methylbutyryl)biphenyl. (yield: 48%) Maintaining the mixed solution at 0° C. stirred for 10 hours at room temperature the organic layer was washed with dil. hydrochloric acid an aquious sodium hydrogen carbonate solution, and then dried with magnesium sulfate The concentrated product was purified by column chromatography

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Then, 4.0 g of (+)-2-methyl butanoyl chloride and 7 ml of nitrobenzene were charged into a flask and cooled to 0° C., added with 10.74 g (80 mmol) of anhydrous aluminum chloride and further with a solution of 4.97 g (19.6 mmol) of (+)-biphenyl-2-methylbutanoate in 9 ml of nitrobenzene, which was stirred at room temperature for 70 hours. After the addition of 2 normal hydrochloric acid and ice, the extraction with chloroform was performed. The extracted chloroform phase was washed with water, dried on anhydrous magnesium sulfate, and the solvent was distilled off. The residue was purified through a column chromatography of silica gel after distillation off of the solvent to obtain 3.60 g (yield: 54%) of an oily (+)-4-(2-methylbutanoyl) biphenyl-2-methylbutanoate. The NMR analytical values of this product were as follows. the extraction with chloroform The extracted chloroform phase was washed with water dried on anhydrous magnesium sulfate the solvent was distilled off The residue was purified through a column chromatography of silica gel after distillation off of the solvent

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

实验步骤: The procedure of Example 3 was followed for the reaction of 60g (0.5 mole) of 2-methylbutyryl chloride with 67g (0.5 mole) of tert-butylbenzene. Obtained was 98.6g of a clear liquid: ir (film) 3.4 (s), 5.95 (s), 8.2 (m) microns; nmr (CDCl3) 7.66 (4H, d of d) 3.37 (1H, q), 1.77 (2H, m), 1.28 (9H, s), 1.16 (3H, d), 0.88 (3H, t) ppm. A VPC analysis indicated a single pure product. Obtained

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Then, 4.0 g of (+)-2-methylbutanoic acid chloride and 7 ml of nitrobenzene were charged into a flask and cooled to 0° C., to which was added 10.74 g (80 mmol) of aluminum chloride with stirring and further added a solution of 4.97 g (19.6 mmol) of (+) 2-methylbutanoic acid-4-biphenyl in 9 ml of nitrobenzene and then stirred at room temperature for 70 hours. Thereafter, the resulting mixture was added with 2 normal hydrochloric acid and ice and extracted with chloroform. The chloroform layer was washed with water, dried on anhydrous magnesium sulfate, and purified by a column chromatography of silica gel after the distillation off of the solvent to obtain 3.60 g (yield 54%) of oily 2-methylbutanoic acid-4-(2-methylbutanoyl) biphenyl. The NMR analytical values of this purified product were as follows. stirred at room temperature for 70 hours extracted with chloroform The chloroform layer was washed with water dried on anhydrous magnesium sulfate purified by a column chromatography of silica gel after the distillation off of the solvent

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

实验步骤: To a suspension of AlCl3 (35.4 g) in CHCl3 (500 mL) at −10° C. was added dropwise 2-methylbutyryl chloride (3.13 g) followed by thioanisole (31.2 mL). The mixture was then stirred at r.t. for 20 min. and was then cooled back to 0° C. Water (200 mL) was then added over 30 min. The CHCl3 layer was separated and dried over MgSO4. After filtration and removal of the solvent, the residue was dried under vacuum at 80° C. for 2 h to give 35 g of the title compound. was then cooled back to 0° C The CHCl3 layer was separated dried over MgSO4 After filtration and removal of the solvent the residue was dried under vacuum at 80° C. for 2 h

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

实验步骤: To a suspension of AlCl3 (35.4 g) in CHCl3 (500 mL) at -10° C. was added dropwise 2-methylbutyryl chloride (31.3 g) followed by thioanisole (31.2 mL). The mixture was then stirred at r.t. for 20 min. and was then cooled back to 0° C. Water (200 mL) was then added over 30 min. The CHCl3 layer was separated and dried over MgSO4. After filtration and removal of the solvent, the residue was dried under vacuum at 80° C. for 2 h to give 35 g of the title compound. was then cooled back to 0° C The CHCl3 layer was separated dried over MgSO4 After filtration and removal of the solvent the residue was dried under vacuum at 80° C. for 2 h

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

实验步骤: To a suspension of AlCl3 (35.4 g) in CHCl3 (500 mL) at -10° C. was added dropwise 2-methylbutyryl chloride (31.3 g) followed by thioanisole (31.2 mL). The mixture was then stirred at r.t. for 20 min. and was then cooled back to 0° C. Water (200 mL) was then added over 30 min. The CHCl3 layer was separated and dried over MgSO4. After filtration and removal of the solvent, the residue was dried under vacuum at 80° C. for 2 h to give 35 g of the title compound. was then cooled back to 0° C The CHCl3 layer was separated dried over MgSO4 After filtration and removal of the solvent the residue was dried under vacuum at 80° C. for 2 h