Synthesis
In a 500 ml four-necked flask equipped with mechanical stirring, constant pressure dropping funnel, reflux condenser and thermometer, 20 g (0.0995 mol) of aminothiazoleacetic acid was added, dibenzothiazole sulfide, pyridine and 100 ml of dichloromethane were added proportionally, stirring was turned on, and 80 ml of dichloromethane solution of triphenylphosphorane was added slowly dropwise at room temperature with vigorous stirring, and then after the addition, it was cooled and dried at 20-25C at a The reaction was stirred at a temperature of 20~25 for 3h(t1), cooled in an ice bath, filtered, and the filter cake was washed with methanol and dried in vacuum to obtain AE-active ester 29.1g (0.08314mol, the theoretical value of 0.0995mol), the yield was 83.6%, and the content was 98.6% (LC); the filtrate was slowly added with a drop of 50ml dichloromethane solution of bis (trichloromethyl) carbonate under vigorous stirring, the filtrate was added slowly at 20~25 with stirring, and the reaction was completed at 20~25 with stirring, and then added slowly at 20~25 with the addition of 80 ml of methylene chloride solution of triphenylphosphine. After addition, the reaction was continued at 20-25 for 3 hours (t2), after the end of the reaction, filtration, the filter cake was washed with methanol, obtained dibenzothiazole sulfide 16.6g (0.05mol, the theoretical value for the recovery of the amount of the amount obtained and the amount of the amount of the reaction did not take part in the sum of the reaction, here it should be 0.0995 1.2-0.0995+0.0995/2=0.07mol), the yield was 71.43 The filtrate was concentrated and recrystallized from methanol to yield 22.9 g of triphenylphosphine (0.0874 mol, the theoretical value is 0.1194 mol) in about 73.2% yield and 98.3% content (LC).
