反应详情

In a three-neck flask they are introduced 7.2g 3-diethylaminopropionic acid (hydrochloride) and 180 ml hexamethylphosphorotriamide. The suspension is cooled with an ice-bath and then 2,90 ml thionylchloride are added while maintaining the inner temperature between +5° - +10° C. The reaction mixture progressively gives a yellow solution. After 2 hours stirring 10.9 g of 2-methoxy 5-morpholinylsulphonyl aniline are added portionwise and the whole mixture is kept under stirring for 4 hours at room temperature and then let to stand for a night. The dark solution is thereafter diluted with 1 l ethyl ether and it appears a precipitate. After 1 hour standing the precipitate is collected, suction-filtered and washed with acetone. After thoroughly drying the raw product weighing 11.3g is recovered and further recrystallised from acetone.

1. temperatureThe suspension is cooled with an ice-bath
2. temperaturewhile maintaining the inner temperature between +5° - +10° C
3. customThe reaction mixture progressively gives a yellow solution
4. additionare added portionwise
5. waitto stand for a night
6. waitAfter 1 hour standing
7. customthe precipitate is collected
8. filtrationsuction-filtered
9. washwashed with acetone
10. dry with materialAfter thoroughly drying the raw product
11. customis recovered
12. customfurther recrystallised from acetone