甲基 2-氯-6-氨磺酰基苯甲酸酯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 100 g of methyl 6-chloro-2-aminosulfonyl-benzoate were suspended in 300 ml of 1,2-dichloroethane, 123 g of thionuyl chloride were added with stirring, and the mixture was slowly heated to the reflux temperature. After it had been stirred for 5 hours under reflux, it was cooled to 55° C., 1.5 ml of pyridine were added and the mixture again heated to the reflux temperature, while introducing phosgene. After 4 hours' treatment with phosgene gas, the reaction mixture was concentrated under reduced pressure and flushed with nitrogen. The oil which remained (105 g) was used, without further purification, for the subsequent stages. the mixture was slowly heated to the reflux temperature After it had been stirred for 5 hours under reflux the mixture again heated to the reflux temperature the reaction mixture was concentrated under reduced pressure flushed with nitrogen was used, without further purification, for the subsequent stages

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 504 g (2.02 mol) of methyl 6-chloro-2-aminosulfonylbenzoate was added in portions to a solution of 80 g (2.0 mol) of sodium hydroxide in 2.5 liters of water; the temperature rose from 25° C. to 50° C. After 30 minutes at this temperature, the mixture was cooled to 25° C. and extracted with methyl tert-butyl ether, and the aqueous phase was stirred into 2N hydrochloric acid. The precipitate was isolated, washed with water and dried. There was obtained 330 g (75.8% of theory) of the title compound, m.p.: 210°-212° C. rose from 25° C. to 50° C extracted with methyl tert-butyl ether The precipitate was isolated washed with water dried

反应条件: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 100 g of methyl 6-chloro-2-aminosulfonyl-benzoate were suspended in 300 ml of 1,2-dichloroethane, 123 g of thionuyl chloride were added with stirring, and the mixture was slowly heated to the reflux temperature. After it had been stirred for 5 hours under reflux, it was cooled to 55° C., 1.5 ml of pyridine were added and the mixture again heated to the reflux temperature, while introducing phosgene. After 4 hours' treatment with phosgene gas, the reaction mixture was concentrated under reduced pressure and flushed with nitrogen. The oil which remained (105 g) was used, without further purification, for the subsequent stages. the mixture was slowly heated to the reflux temperature After it had been stirred for 5 hours under reflux the mixture again heated to the reflux temperature the reaction mixture was concentrated under reduced pressure flushed with nitrogen was used, without further purification, for the subsequent stages