Barium hydroxide, octahydrate → HCID 131733076, compound

HRID 2201654Notes

Reaction equation

HRID 2201654 reaction equation
[OH2:1].[NH2:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10](=[O:16])/[CH:11]=[CH:12]\[C:13]([OH:15])=[O:14])=[CH:5][CH:4]=1.O.O.O.O.O.O.O.O.[OH-].[Ba+2:26].[OH-]>O>[OH2:14].[OH2:1].[NH2:2][C:3]1[CH:4]=[CH:5][C:6]([NH:9][C:10](=[O:16])/[CH:11]=[CH:12]\[C:13]([O-:15])=[O:14])=[CH:7][CH:8]=1.[NH2:2][C:3]1[CH:4]=[CH:5][C:6]([NH:9][C:10](=[O:16])/[CH:11]=[CH:12]\[C:13]([O-:15])=[O:14])=[CH:7][CH:8]=1.[Ba+2:26]

Participants

4

Reactant 2

HCID 17749109Barium hydroxide, octahydrateHCID 86708816HCID 86708816, compound

Product 1

HCID 131733076HCID 131733076, compoundYield 142.9%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

Under a nitrogen atmosphere, into a reaction vessel were charged 10.0 g (44.6 mmol) of (2Z)-4-[(4-aminophenyl)amino]-4-oxo-2-butenoic acid mono-hydrate obtained by the same method as in Production Example 2 and 70 ml of water, a solution prepared by dissolving 7.04 g (22.3 mmol) of barium hydroxide octa-hydrate in 30 ml of water was added at 20 to 30° C., and the mixture was stirred at room temperature for 2 hours. Thereafter, the mixture was condensed under reduced pressure and the solvent was distilled off to obtain a residue to which 50 ml of ethanol and 50 ml of 2-propanol were added, and the mixture was stirred at room temperature overnight, the deposited crystal was isolated by filtration, and dried under reduced pressure at 45° C., to obtain 12.4 g of barium bis{(2Z)-4-[(4-aminophenyl)amino]-4-oxo-2-butenoate}di-hydrate as a yellow solid. Yield: 98.3%.

Workup

  1. customa solution prepared
  2. additionwas added at 20 to 30° C.
  3. customcondensed under reduced pressure
  4. distillationthe solvent was distilled off
  5. customto obtain a residue to which 50 ml of ethanol and 50 ml of 2-propanol
  6. additionwere added
  7. stirringthe mixture was stirred at room temperature overnight
  8. customthe deposited crystal was isolated by filtration
  9. customdried under reduced pressure at 45° C.

Sources & evidence

ORD record
ord-4ffc4385f9ab46c9976aaa9a09f905bd
Source dataset
uspto-grants-2016_06
Patent number
US09365497B2

Reaction notes

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