Methane → HCID 131715127, compound

Into a 12-L flask equipped with stirrer, thermometer, additional funnel was charged 528 g L-ascorbic acid (3.0 moles) and 7500 mL distilled water. The batch was stirred at room temperature to form a clear solution and added 600 g calcium carbonate. The slurry was stirred and cooled to 15° C. Then 1200 mL hydrogen peroxide (30% w/w) was added at 12°-15° C. over 60 min. The mixture was stirred at room temperature for 16 h. Then 120 g charcoal was added. The mixture was heated to 75° C. while stirring was continued until no more oxygen was evolved (as indicated by bubbling in a water trap). The batch was filtered at 70°-75° C., and the filter cake washed with 2×100 mL distilled water. The combined filtrate was concentrated to about 2-L at less than 50° C. under vacuum. Then 1500 mL methanol was added until the solution became cloudy. The mixture was then stirred at room temperature for 16 h, filtered, and washed with 2×100 mL methanol. The solids were dried at 60° C. under vacuum to constant weight to obtain calcium-L-threonate monohydrate having a dry weight of 436.5 g and a melting point 300+° C.

1. customInto a 12-L flask equipped with stirrer
2. distillationdistilled water
3. customto form a clear solution
4. stirringThe slurry was stirred
5. temperaturecooled to 15° C
6. stirringThe mixture was stirred at room temperature for 16 h
7. temperatureThe mixture was heated to 75° C.
8. stirringwhile stirring
9. custom(as indicated by bubbling in a water trap)
10. filtrationThe batch was filtered at 70°-75° C.
11. washthe filter cake washed with 2×100 mL
12. distillationdistilled water
13. concentrationThe combined filtrate was concentrated to about 2-L at less than 50° C. under vacuum
14. additionThen 1500 mL methanol was added until the solution
15. stirringThe mixture was then stirred at room temperature for 16 h
16. filtrationfiltered
17. washwashed with 2×100 mL methanol
18. customThe solids were dried at 60° C. under vacuum to constant weight

ORD record

ord-94d25cf00b454fc4859d19fddf6df619

Source dataset

uspto-grants-1987_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04663469