反应详情

A solution of 3.93 gm of m-AMSA and 5.15 gm of D-gluconic acid-water solution (38% w/w) in 305 ml of specially denatured 3A anhydrous ethanol at 70°-80° C. is filtered with suction. The filtrate is cooled to 30°-35° C. and 100 ml of anhydrous diethyl ether is added with stirring. After chilling to 0°-5° C. with stirring, the mixture is stored about 16 hours at 5° C. The product is collected, washed with specially denatured 3A anhydrous ethanol and anhydrous diethyl ether (3:1) at 5° C., then with several portions of anhydrous ether and dried under reduced pressure at 50°-55° C. to give 3.95 gm of m-AMSA D-gluconate. The salt obtained by this process retains a small amount (about 1% of ethanol).

1. customat 70°-80° C.
2. filtrationis filtered with suction
3. temperatureThe filtrate is cooled to 30°-35° C.
4. addition100 ml of anhydrous diethyl ether is added
5. temperatureAfter chilling to 0°-5° C.
6. stirringwith stirring
7. customThe product is collected
8. washwashed
9. customat 5° C.
10. dry with materialwith several portions of anhydrous ether and dried under reduced pressure at 50°-55° C.