氯雷他定杂质69

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: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: A mixture of 628 mg of dimethyl aminoterephthalate, 546 mg of 3-chlorophenylacetonitrile and 15 mL of 4N hydrogen chloride dioxane solution was stirred at room temperature for 7 hours. Further continuing the stirring at 30° C. for 63 hours and at 70° C. for 25 hours, ice was added to the reaction mixture, followed by addition of 7 mL of 25% aqueous ammonia. Whereupon precipitated crystals were recovered by filtration, and washed with water, ether and chloroform by the order stated. Subjecting the crystals to through-flow drying under heating, 670 mg of the title compound was obtained. stirring at 30° C. for 63 hours at 70° C. for 25 hours ice was added to the reaction mixture Whereupon precipitated crystals were recovered by filtration washed with water, ether and chloroform by the order to through-flow drying under heating

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

实验步骤: Starting with 75.0 g (0.495 mol) of 3-chlorobenzyl cyanide, 160.58 g (0.743 mol) of diethyl 3,3-dimethylglutarate, 14.80 g (0.643 mol) of sodium, and 260 ml of dry ethanol a total of 108.08 g (71% yield) of the desired product was obtained using the procedure described in Example I, Part A.

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

实验步骤: Sodium hydroxide (0.62 mol) was dissolved in methanol (100 ml) and the mixture was cooled till room temperature. 1-bromo-4-nitro-benzene (0.124 mol), followed by 3-chloro-benzeneacetonitrile (0.223 mol) were added dropwise, the temperature raised till 50° C. and the mixture was stirred at room temperature for one night. The mixture was poured into water and ice, the precipitate was filtered off, washed with water and extracted with CH2Cl2 and CH3OH. The organic layer was dried (MgSO4), filtered off and evaporated till dryness. The residue was taken up in Et2O, filtered off and dried, yielding 13.2 g (34.8%) of 5-bromo-3-(3-chlorophenyl)-2,1-benzisoxazole, mp. 163° C. (intermediate 1). were added dropwise the temperature raised till 50° C. the precipitate was filtered off washed with water extracted with CH2Cl2 and CH3OH The organic layer was dried (MgSO4) filtered off evaporated till dryness filtered off dried

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir: