反应详情

温度

80 °C

To a mixture of 5.6 g. (0.03 mole) of thieno[3,4-d]isothiazol-3(2H)-one 1,1-dioxide* in 50 ml. of dry pyridine is added 5.6 g. (0.016 mole) of phosphorus pentasulfide portionwise over 3 minutes. The viscous mixture is slowly heated in an oil bath under an atmosphere of nitrogen. The temperature of the oil bath is slowly increased to 80° C. after 30 minutes. The temperature of the oil bath is then kept at 80° C. for 25 minutes, the internal temperature reading 63° C. The solution is cooled to 50° C. and is added dropwise over 5 minutes to 200 ml. of water and cooled in an ice bath. The precipitate which forms is collected and discarded. The filtrate is cooled in ice and acidified with concentrated hydrochloric acid to pH 1. The precipitate which forms is collected to yield 40% of material. In another expeirment, a sample is recrystallized from water to obtain an analytical sample, m.p. 196°-8° C. (dec.).

1. additionTo a mixture of 5.6 g
2. temperatureThe viscous mixture is slowly heated in an oil bath under an atmosphere of nitrogen
3. customreading 63° C
4. temperatureThe solution is cooled to 50° C.
5. additionis added dropwise over 5 minutes to 200 ml
6. customThe precipitate which forms is collected
7. temperatureThe filtrate is cooled in ice
8. customThe precipitate which forms is collected