1,1,2-trichloroethane

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:

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

実験手順: To a mixture of 1155 grams of dichloromethane and 493.5 grams of 1,1,2-trichloroethane was added 8.04 grams of 4-((4-dimethylaminophenyl)-2,6diphenyl)-6-phenyl thiapyrylium tetrafluoroboiate and 5.36 grams of 4-(4dimethylaminophenyl)-2-(4-ethoxyphenyl)-6-phenyl thiapyrylium tetrafluoroborate. The mixture was stirred mechanically for one hour; to the resulting solution was added 102 grams of high molecular weight bisphenol A polycarbonate, (Makrolon™ 5705 polycarbonate, obtained from Mobay Chemical Co.). After one houl additional stiiling, 238 grams of bisphenol A polycaibonate of lower molecular weight (Lexan 145™ polycarbonate, obtained from General Electric Co.) was added. The mixture was stirred ovemnight, then diluted with 211.5 grams of 1,1,2-tuichloroethane. The resulting slulTy was allowed to evaporate to dryness, and the residue was cut into small pieces. The high molecular weight polycarbonate referred to above was Makrolon 5705™ polycarbonate, obtained from Mobay Chemical Co. Its number average molecular weight, as determined by gel permeation chromatography, is 178,000 polystyrene equivalents. The low molecular weight polycarbonate above was Lexan 145™ polycarbonate, obtained from General Electric Co. Its number average molecular weight as determined by gel permeation chromatography is 51,600 polystyrene equivalents.

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: A solution of 1.43 g. of p-nitrobenzyl 6β-formamido-2,2-dimethylpenam-3-carboxylate-1-oxide and 500 mg. of N-chlorosuccinimide in 40 ml. of dry 1,1,2-trichlorethane was refluxed for 90 minutes. The mixture was cooled, washed with water and brine, dried over MgSO4, and the solvent was evaporated. The nmr spectrum indicates conversion to the title compound. The mixture was cooled washed with water and brine dried over MgSO4 the solvent was evaporated

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

実験手順: A solution of 1.43 g. of p-nitrobenzyl 6β-formamido-2,2-dimethylpenam-3-carboxylate-1-oxide and 500 mg. of N-chlorosuccinimide in 40 ml. of dry 1,1,2-trichlorethane was refluxed for 90 minutes. The mixture was cooled, washed with water and brine, dried over MgSO4, and the solvent was evaporated. The nmr spectrum indicates conversion to the title compound. The mixture was cooled washed with water and brine dried over MgSO4 the solvent was evaporated