HRID649144

反应详情

EQUATION

反应方程式

HRID 649144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added dropwise
  2. washwashed with deionized water until no Cl-
  3. customAfter drying in the air
  4. customgrinding
  5. customthe crystals were dried in vacuum at 40° for 20 h