2-[4-(2-methylpropyl)phenyl]acetyl chloride

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 3.5 g of p-isobutylphenylacetic acid chloride in 5.9 g of 2-methoxyethanol was added 1.6 g of triethylamine, and the mixture was stirred at room temperature for 4 hours. After the reaction was complete, an inorganic substance produced was filtered off. The filtrate was extracted with ether, and the extract was washed, dehydrated and applied over a column of silica gel. The adsorbates was eluted with ether, and the eluates were freed of ether to give an oily product. Distillation of the product in vacuo gave 2.8 g of p-isobutylphenylacetic acid-2-methoxyethyl ester as a colorless oil, boiling at 97°-98° C./1 mmHg. Analysis-Calculated for C15H22O3 : C, 71.97; H, 8.86. Found: C, 71.63; H, 8.90. Mass spectrum: parent ion 250 m/e. an inorganic substance produced was filtered off The filtrate was extracted with ether the extract was washed The adsorbates was eluted with ether to give an oily product Distillation of the product in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.5 g (0.028 moles) of carnitine hydrochloride are dissolved in 9 mls of CF3COOH, and to the solution an excess (20 mls) of p-isobutylphenyl acetyl chloride is added and the mixture is kept under stirring at 40°-45° C. for 4-5 hours. At the end of this period of time the mixture is partitioned with H2O--CHCl3, the organic phase is discarded and the aqueous phase is concentrated at reduced pressure at a bath temperature of about 50° C. A gelatinous raw material is obtained which is crystallized with isopropanol, the precipitate thus obtained is filtered, rapidly washed with ether because of its hygroscopicity, and dried under vacuum at a temperature not exceeding 50° C.; 6.8 g of a product are obtained (yield 65%) having the following characteristics: At the end of this period of time the mixture is partitioned with H2O--CHCl3 the aqueous phase is concentrated at reduced pressure at a bath temperature of about 50° C A gelatinous raw material is obtained which is crystallized with isopropanol the precipitate thus obtained is filtered rapidly washed with ether because of its hygroscopicity dried under vacuum at a temperature not exceeding 50° C.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 3.5 g of p-isobutylphenylacetic acid chloride in 5.9 g of 2-methoxyethanol was added 1.6 g of triethylamine, and the mixture was stirred at room temperature for 4 hours. After the reaction was complete, an inorganic substance produced was filtered off. The filtrate was extracted with ether, and the extract was washed, dehydrated and applied over a column of silica gel. The adsorbates was eluted with ether, and the eluates were freed of ether to give an oily product. Distillation of the product in vacuo gave 2.8 g of p-isobutylphenylacetic acid-2-methoxyethyl ester as a colorless oil, boiling at 97°-98° C./1 mmHg. Analysis-Calculated for C15H22O3 : C, 71.97; H, 8.86. Found: C, 71.63; H, 8.90. Mass spectrum: parent ion 250 m/e. an inorganic substance produced was filtered off The filtrate was extracted with ether the extract was washed The adsorbates was eluted with ether to give an oily product Distillation of the product in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 3.5 g of p-isobutylphenylacetic acid chloride in 5.9 g of 2-methoxyethanol was added 1.6 g of triethylamine, and the mixture was stirred at room temperature for 4 hours. After the reaction was complete, an inorganic substance produced was filtered off. The filtrate was extracted with ether, and the extract was washed, dehydrated and applied over a column of silica gel. The adsorbates was eluted with ether, and the eluates were freed of ether to give an oily product. Distillation of the product in vacuo gave 2.8 g of p-isobutylphenylacetic acid-2-methoxyethyl ester as a colorless oil, boiling at 97°-98° C./1 mmHg. Analysis-Calculated for C15H22O3 : C, 71.97; H, 8.86. Found: C, 71.63; H, 8.90. Mass spectrum: parent ion 250 m/e. an inorganic substance produced was filtered off The filtrate was extracted with ether the extract was washed The adsorbates was eluted with ether to give an oily product Distillation of the product in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.5 g (0.028 moles) of carnitine hydrochloride are dissolved in 9 mls of CF3COOH, and to the solution an excess (20 mls) of p-isobutylphenyl acetyl chloride is added and the mixture is kept under stirring at 40°-45° C. for 4-5 hours. At the end of this period of time the mixture is partitioned with H2O--CHCl3, the organic phase is discarded and the aqueous phase is concentrated at reduced pressure at a bath temperature of about 50° C. A gelatinous raw material is obtained which is crystallized with isopropanol, the precipitate thus obtained is filtered, rapidly washed with ether because of its hygroscopicity, and dried under vacuum at a temperature not exceeding 50° C.; 6.8 g of a product are obtained (yield 65%) having the following characteristics: At the end of this period of time the mixture is partitioned with H2O--CHCl3 the aqueous phase is concentrated at reduced pressure at a bath temperature of about 50° C A gelatinous raw material is obtained which is crystallized with isopropanol the precipitate thus obtained is filtered rapidly washed with ether because of its hygroscopicity dried under vacuum at a temperature not exceeding 50° C.