Sodium Hydroxide → HCID 178488037, compound

HRID 888166Notes

Reaction equation

HRID 888166 reaction equation
[CH3:1][C:2]1[CH:3]=[N:4][C:5]([CH2:11][S+:12]([O-:24])[C:13]2[NH: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].[OH-].[Na+:26]>C(O)C>[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].[Na+:26]

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 178488147HCID 178488147, compound

Product 1

HCID 178488037HCID 178488037, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

According to the present invention omeprazole sodium ethanol solvate is prepared by dissolving omeprazole (base) in a solution of NaOH in absolute ethanol. Mechanical particles are removed from the resulting solution, e.g. by filtration, and further seeded with crystals of omeprazole sodium form A to induce crystallisation. The slurry is then agitated for several hours at ambient temperature and additionally for several hours at low temperatures, e.g. from 0° to 5° C., in order to improve the yield. The precipitated omeprazole sodium form A is separated, e.g. by filtration or centrifugation, and washed with cooled absolute ethanol. Omeprazole sodium ethanol wet thus derived is dried under reduced pressure from 40° to 50° C., preferably at about 45° C. to yield stable anhydrous omeprazole sodium in ethanol solvate form. By the term “omeprazole sodium ethanol wet” is meant the product obtained before the step of drying under reduced pressure. The term “reduced pressure” generally refers to a pressure of about 10 mbar to about 50 mbar.

Workup

  1. customis prepared
  2. customMechanical particles are removed from the resulting solution, e.g. by filtration
  3. customcrystallisation
  4. customThe precipitated omeprazole sodium form A is separated
  5. filtratione.g. by filtration or centrifugation
  6. washwashed
  7. temperaturewith cooled absolute ethanol
  8. dry with materialOmeprazole sodium ethanol wet thus derived is dried under reduced pressure from 40° to 50° C., preferably at about 45° C.

Sources & evidence

ORD record
ord-7f6c1055fd4845909ab7c4ba48cd4521
Source dataset
uspto-grants-2012_08
Patent number
US08247566B2

Reaction notes

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