Magnesium Sulfate Heptahydrate → HCID 49800017, compound

HRID 1952197Notes

Reaction equation

HRID 1952197 reaction equation
[CH3:1][C:2]1[CH:3]=[N:4][C:5]([CH2:11][S+:12]([O-:24])[C:13]2[N-:14][C:15]3[CH:16]=[CH:17][C:18]([O:22][CH3:23])=[CH:19][C:20]=3[N:21]=2)=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9].[K+].O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Mg+2:38]>CO>[CH3:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([CH3:10])[C:5]([CH2:11][S@@:12]([C:13]2[N-:14][C:15]3[CH:16]=[CH:17][C:18]([O:22][CH3:23])=[CH:19][C:20]=3[N:21]=2)=[O:24])=[N:4][CH:3]=1.[Mg+2:38]

Participants

4

Reactant 2

HCID 24843Magnesium Sulfate HeptahydrateHCID 178488036HCID 178488036, compound

Product 1

HCID 49800017HCID 49800017, compoundYield 45%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
2.5 °C

Procedure

To a solution of esomeprazole potassium salt (100 g, 0.261 mole) in methanol (500 ml) kept in a round bottom flask, was added magnesium sulphate heptahydrate (64.1 g, 0.26 mole) at 25-30° C. and stirred for 1.5-2 hrs. The insoluble material formed was filtered off and the filtrate was passed through a 0.45 micron membrane filter. To the filtrate, water (1300 ml) was added and stirred at 25-30° C. for 1-1.5 hrs, cooled to 0-5° C., and stirred for a further period of 1-1.5 hrs. The solid formed was collected by filtration and washed with water and dried under reduced pressure at 40-45° C. to obtain the esomeprazole magnesium salt.

Workup

  1. customThe insoluble material formed
  2. filtrationwas filtered off
  3. filtrationfilter
  4. additionTo the filtrate, water (1300 ml) was added
  5. stirringstirred at 25-30° C. for 1-1.5 hrs
  6. stirringstirred for a further period of 1-1.5 hrs
  7. customThe solid formed
  8. filtrationwas collected by filtration
  9. washwashed with water
  10. customdried under reduced pressure at 40-45° C.

Sources & evidence

ORD record
ord-ad39d2d0569c46969d799cd9cab5d313
Source dataset
uspto-grants-2013_03
Patent number
US08404853B2

Reaction notes

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