反应详情

Air was sparged at 100 mL/min through a rapidly stirred solution of potassium hydroxide (41.9 g, 65.5 mmol) and D-galactose (45.0 g, 25.0 mmol) in a mixture of methanol/water (375 mL/180 mL) at 60 psi in a Parr bomb (1 L). The temperature was maintained at 35°-36° C. throughout the reaction. After sparging for 24 hours (h), methanol (50 mL) was added and sparging continued for a total of 45 h. The reaction mixture was cooled and vented. The bomb was opened and the light yellow mixture was filtered to remove a small amount of solids. The bomb and filter were rinsed with water (5 mL) in which most of the solids dissolved. The filtrate was stirred and diluted with methanol (850 mL). Crystallization occurred after approximately 500 mL of methanol had been added. After stirring for 4 h, the crystals were collected by filtration and vacuum dried to provide 29.3 g (57% yield) of potassium D-lyxonate 1 as a white solid: DISC mp 171.25° C.; Analysis calculated for C5H9O6K: C, 29.41; H, 4.44. Found: C, 28.86; H, 4.16. This white solid material was used in Example 2 without further purification.

1. temperatureThe temperature was maintained at 35°-36° C. throughout the reaction
2. customAfter sparging for 24 hours (h), methanol (50 mL)
3. additionwas added
4. customsparging
5. customcontinued for a total of 45 h
6. temperatureThe reaction mixture was cooled
7. filtrationthe light yellow mixture was filtered
8. customto remove a small amount of solids
9. filtrationThe bomb and filter
10. washwere rinsed with water (5 mL) in which most of the solids
11. dissolutiondissolved
12. additiondiluted with methanol (850 mL)
13. customCrystallization
14. additionhad been added
15. stirringAfter stirring for 4 h
16. filtrationthe crystals were collected by filtration and vacuum
17. customdried