Methane → HCID 178495389, compound

HRID 888248Notes

Reaction equation

HRID 888248 reaction equation
[CH3:1][C:2]1[C:7]([CH2:8][S+:9]([O-:19])[C:10]2[NH:11][C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=3[N:18]=2)=[N:6][CH:5]=[CH:4][C:3]=1[O:20][CH2:21][CH2:22][CH2:23][O:24][CH3:25].[OH-].[Na+:27].C>O>[CH3:1][C:2]1[C:7]([CH2:8][S+:9]([O-:19])[C:10]2[N-:11][C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=3[N:18]=2)=[N:6][CH:5]=[CH:4][C:3]=1[O:20][CH2:21][CH2:22][CH2:23][O:24][CH3:25].[Na+:27]

Participants

5

Reactant 3

HCID 297MethaneHCID 14798Sodium HydroxideHCID 178495390HCID 178495390, compound

Product 1

HCID 178495389HCID 178495389, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
27.5 °C

Procedure

Rabeprazole (10 g) was suspended in 20 ml water and sodium hydroxide solution (1.11 g sodium hydroxide dissolved in 10 ml water) was added at 25-30° C. Reaction mass was stirred for 30 minutes at 25-30° C. Added activated charcoal (1.0 g) and stirred for 30 minutes at 25-30° C. Filtered and washed charcoal bed with water (10 ml). Added 30 ml ethanol to filtrate and distilled out till get oily residue under reduced pressure at 30-35° C. Again added 30 ml ethanol to the oily residue and distilled out completely under reduced pressure at 35° C. To the residue added 100 ml diisopropyl ether and stirred at 25-30° C. for two hours. Filtered product under nitrogen atmosphere and washed with 20 ml diisopropyl ether. Dried under vacuum at 50° C. for 20-24 hours to obtain amorphous Rabeprazole sodium.

Workup

  1. customReaction mass
  2. stirringstirred for 30 minutes at 25-30° C
  3. filtrationFiltered
  4. washwashed charcoal bed with water (10 ml)
  5. additionAdded 30 ml ethanol to filtrate
  6. distillationdistilled out
  7. customtill get oily residue under reduced pressure at 30-35° C
  8. distillationAgain added 30 ml ethanol to the oily residue and distilled out completely under reduced pressure at 35° C
  9. additionTo the residue added 100 ml diisopropyl ether
  10. stirringstirred at 25-30° C. for two hours
  11. washFiltered product under nitrogen atmosphere and washed with 20 ml diisopropyl ether
  12. customDried under vacuum at 50° C. for 20-24 hours

Sources & evidence

ORD record
ord-4daa7524e8474e809b0dc79048c263ac
Source dataset
uspto-grants-2012_08
Patent number
US08247568B2

Reaction notes

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