(甲基硫代)乙腈

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:

反应条件: temp:-70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 4.0 ml (0.088 mole) of chlorine in 200 ml of methylene chloride cooled to -70° C. is added dropwise a solution of 7.65 g (0.088 mole) of methylthioacetonitrile in 1 liter of methylene chloride while maintaining the temperature below -65° C. After several minutes a solution containing 0.2 mole of 2-amino-5-methoxybenzophenone in 100 ml of methylene chloride is added dropwise over a 30 min period. The mixture is stirred at -70° C. for about 1.5 hr and 18 g (0.18 mole) of triethylamine is added. The mixture is stirred for about an hour at -70° C. and then allowed to warm to ambient temperature. The mixture is washed with water, dried over sodium sulfate and concentrated under reduced pressure. The residue is recrystallized from a suitable solvent, e.g., 2-propanol, to give the title product. while maintaining the temperature below -65° C is added dropwise over a 30 min period The mixture is stirred for about an hour at -70° C. to warm to ambient temperature The mixture is washed with water dried over sodium sulfate concentrated under reduced pressure The residue is recrystallized from a suitable solvent, e.g., 2-propanol

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

实验步骤: To a solution of 46.3 g (0.2 mole) of 4'-chloro-2-aminobenzophenone and 17.4 g (0.2 mole) of methylthioacetonitrile in 1 liter of methylene dichloride at a temperature of -70° C. was added dropwise 22.2 g (0.21 mole) of tert. butyloxychloride at a rate to ensure that the reaction temperature did not exceed -65° C. The resulting solution was allowed to warm to ambient temperature, washed twice with water, dried over sodium sulphate, and concentrated to give a gum residue. The gum crystallized when it was triturated with diethyl ether. The solid was collected by filtration and recrystallized from 2-propanol to yield 43.0 g (68%) of the title compound as a tan solid, m.p. 122° C. did not exceed -65° C washed twice with water dried over sodium sulphate concentrated to give a gum residue The gum crystallized when it was triturated with diethyl ether The solid was collected by filtration recrystallized from 2-propanol

反应条件: temp:-69.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a slurry of 29.6 g (0.15 mole) of 2-aminobenzophenone and 13.1 g (0.15 mole) of (methylthio)acetonitrile in 400 ml of methylene dichloride at a temperature of -68° C. was added dropwise 16.8 g (0.155 mole) of t-butyloxychloride at a rate to ensure that the reaction temperature did not exceed -64° C. The resulting solution was stirred at -69° C. for one hour, treated with 15.7 g (0.155 mole) of triethylamine and allowed to warm to ambient temperature. The solution obtained was washed twice with water, dried over sodium sulphate, and concentrated to give 45.2 g of a dark oil as the residue. This residue was chromatographed on 1 kg of silica gel to yield 22.5 g (53%) of the title compound as tan crystals, m.p. 107°-108° C. did not exceed -64° C to warm to ambient temperature The solution obtained was washed twice with water dried over sodium sulphate concentrated