反应详情

11.9g. of calcium pantothenate, 5.6g. of cystamine dihydrocloride and 7.7g. of 1-hydroxybenzotriazole were dissolved in a mixed solvent of 50ml. of pyridine, 10ml. of water and 25ml. of benzene, and thereafter pyridine (25ml.) solution of 10.5g. of dicyclohexylcarbodiimide was added thereto at a time, and then this was subjected to reaction at a temperature below 10° C for 1 hour and thereafter to reaction at a room temperature for 5 hours. Then the solvent was removed at a reduced pressure, and the residue thereof was added with 50ml. of water and the resultant deposited crystals were removed by filtration. Pyridine left in the filtered mother liquor was completely removed azeotropically with water. The residue thereof was added with 50ml. of water, and after cooling it, the deposited crystals was removed by filtration, and extracted two times with 20ml. of chloroform. The water layer was passed through a monobed column composed of 78ml. of strong acidic cation exchanger resin (Amberlite 1R-120B) [H+] and 150ml. of strong basic anion exchanger resin (Amberlite 1RA-410) [OH-], and washed out with water. The presence of the objective compound in the flowed out liquid was traced by refractometer. The eluted solution was concentrated under a reduced pressure and subjected to freeze drying, and thereby 9.6g. of pantethine in the form of pulverized crystal was obtained (69.2% yield).

1. customat a time, and then this was subjected to reaction at a temperature below 10° C for 1 hour
2. customto reaction at a room temperature for 5 hours
3. customThen the solvent was removed at a reduced pressure
4. additionthe residue thereof was added with 50ml
5. customwere removed by filtration
6. waitPyridine left in the filtered mother liquor
7. customwas completely removed azeotropically with water
8. additionThe residue thereof was added with 50ml
9. temperatureof water, and after cooling it
10. customthe deposited crystals was removed by filtration
11. extractionextracted two times with 20ml
12. washof strong basic anion exchanger resin (Amberlite 1RA-410) [OH-], and washed out with water
13. concentrationThe eluted solution was concentrated under a reduced pressure
14. customto freeze drying