HRID649144
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Anhydrous CaCl2 (17.9 g, 0.161 mol) dissolved in deionized water (200 ml) was added dropwise under viogorous stirring to a solution of omeprazole sodium salt (125 g, 0.340 mole) in deionized water (1250 ml) and then stirring was continued for 1 h at room temperature. The precipitate was centrifuged down and washed with deionized water until no Cl- was detectable (AgNO3). After drying in the air and grinding, the crystals were dried in vacuum at 40° for 20 h yielding omeprazole calcium salt dihydrate (104 mg, 80%), mp 182°-184° C., NMR: δ(CDCl3 1 drop of DMSO-d6) 2.0(s, 3H), 2.15(s, 3H), 3.6(s, 3H), 3.7(s, 3H), 4.5(s, 2H), 6.7(dd, 1H), 7.1(d, 1H), 7.6(d, 1H, 8.15(s, 1H).
WORKUP
后处理
- additionwas added dropwise
- washwashed with deionized water until no Cl-
- customAfter drying in the air
- customgrinding
- customthe crystals were dried in vacuum at 40° for 20 h