* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Example 8 Preparation of (6S)-calcium folinate starting from the mother liquors of example 6. 80 g of calcium chloride dihydrate are added to the mother liquors of example 6. After addition of 900 g of ethanol, the solution is kept under stirring for 30 min, the precipitate is filtered, and washed with 40 g of ethanol. The product is dried, then redissolved in water and reprecipitated at pH 7 by addition of ethanol. 16 g of (6S)-calcium folinate, 75% optically pure, are obtained. The product is recrystallized three times from water, at pH 7 and in the presence of ~4 parts by weight of calcium chloride dihydrate. After dissolution in water and precipitation with ethanol, 5 g of (6S)-calcium folinate, with an optical purity higher than 99%, are obtained.
1. Crystallization 100 g crude calcium-(6R,S)-folinate in approximately 1 liter of warm water at 50-60 C. are treated with 12-36 g calcium chloride (CaCl2.2H2 O), adjusted to a pH of 10 at 30 C. by the addition of aqueous ammonia (25%) and allowed to crystallize at 18 C. After 18-20 hours the precipitated product is filtered off, washed with dilute calcium chloride solution and then with moistened ethanol. 41 g calcium folinate are obtained containing 88% calcium-(6S)-folinate and 12% calcium-(6R)-folinate.
3
[ 6035-45-6 ]
leucovorin zinc[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
2.5 g
With zinc acetate dihydrate; In water; at 40℃;
4.0 g of <strong>[6035-45-6]leucovorin calcium</strong> (6.7 mmol) are suspended in 100 ml water. The slurry is heated up to about 40Cto get a clear solution. 1.0 g of zinc acetate dihydrate (4.6 mmol) in 10 ml water is slowly added. A precipitate is formedimmediately. After one day the precipitate is separated from the mother liquor. Yield: 2.5 g leucovorin zinc (4.0 mmol),almost insoluble in water.