benzoyl cyanide

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: There were present in a stirrer equipped apparatus protected against moisture, 131 grams (1.0 mole) of benzoyl cyanide, 148 grams (2.0 moles) of t-butanol and 50 ml of methylene chloride and under stirring at about +50° C. it was treated by dropwise addition 150 grams (1.5 moles) of concentrated sulfuric acid. After the end of the dropping, the mixture was post-stirred for another hour at room temperature and then the entire mixture poured on 400 grams of ice and well agitated. Subsequently, the mixture was extracted with methylene chloride and the methylene chloride solution evaporated. There resulted 195 grams of phenylglyoxylic-N-t-butylamide which corresponds to a yield of 95% based on the acyl cyanide added. The amide has a melting point of 76°-77° C. There were present in a stirrer equipped apparatus After the end of the dropping, the mixture was post-stirred for another hour at room temperature well agitated Subsequently, the mixture was extracted with methylene chloride the methylene chloride solution evaporated

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

実験手順: 72 g (0.5 mol) of sodium benzoate were mixed with 140.6 g (1 mol) of benzoyl chloride and 80 ml of tetramethylene-sulphone and 25 g (0.5 mol) of 98% pure sodium cyanide. After a stirring time of 20 minutes, an exothermic rise in the temperature to 85° C. was observed. It was now easier to stir the mixture. The subsequent reaction time was 2.5 hours at 150°-160° C. Working up gave the following yield: 65 g (99.3% of theory) of benzoyl cyanide; melting point 34° C. After a stirring time of 20 minutes to 85° C.

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

実験手順: 72 g (0.5 mol) of sodium benzoate were mixed with 140.6 g (1 mol) of benzoyl chloride and 80 ml of tetramethylene-sulphone and 25 g (0.5 mol) of 98% pure sodium cyanide. After a stirring time of 20 minutes, an exothermic rise in the temperature to 85° C. was observed. It was now easier to stir the mixture. The subsequent reaction time was 2.5 hours at 150°-160° C. Working up gave the following yield: 65 g (99.3% of theory) of benzoyl cyanide; melting point 34° C. After a stirring time of 20 minutes to 85° C.

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

実験手順: Benzoyl cyanide, 0.67 g (0.005 mole) and methyl 1-methylpyrrole-2-acetate, 0.76 g (0.005 mole) were stirred together in ether (2 ml) containing oxalic acid (0.04 g). The reaction was run in the dark at room temperature. After six days, the reaction mixture was placed in the freezer overnight, filtered, and washed with cold ether to yield 0.17 g (12 percent) of methyl 1-methyl-5-(cyanohydroxyphenylmethyl)pyrrole-2-acetate, mp 137°-8°. The solid state IR spectrum was identical to authentic material. dark at room temperature was placed in the freezer overnight filtered washed with cold ether

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

実験手順: A solution of 6.7 g (0.05 mole) of benzoylcyanide, 7.6 g (0.05 mole) of methyl 1-methylpyrrole-2-acetate and 0.2 g of trichloroacetic acid in 20 ml. of ether was stirred for four days at 25° C. under argon. The solution was cooled to 0° and the solid methyl 5-(cyanohydroxyphenylmethyl)-1-methylpyrrole-2-acetate was collected by filtration; mp 148°-153°, yield, 4.0 g (28 percent). The solution was cooled to 0° the solid methyl 5-(cyanohydroxyphenylmethyl)-1-methylpyrrole-2-acetate was collected by filtration mp 148°-153°, yield

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

実験手順: A solution of 6.7 g (0.05 mole) of benzoylcyanide, 7.6 g (0.05 mole) of methyl 1-methylpyrrole-2-acetate and 0.2 g of trichloroacetic acid in 20 ml. of ether was stirred for four days at 25° C. under argon. The solution was cooled to 0° and the solid methyl 5-(cyanohydroxyphenylmethyl)-1-methylpyrrole-2-acetate was collected by filtration; mp 148°-153°, yield, 4.0 g (28 percent). The solution was cooled to 0° the solid methyl 5-(cyanohydroxyphenylmethyl)-1-methylpyrrole-2-acetate was collected by filtration mp 148°-153°, yield