Sodium Sulfate → HCID 19096401, compound

HRID 486711Notes

Reaction equation

HRID 486711 reaction equation
[Br:1][C:2]1[S:6][C:5]([CH:7]=O)=[CH:4][CH:3]=1.[CH3:9][C:10](=[O:15])[CH2:11][C:12](=[O:14])[CH3:13].[O-]S([O-])(=O)=O.[Na+].[Na+]>CC(O)C.S(Cl)(Cl)=O>[Br:1][C:2]1[S:6][C:5]([CH:7]=[C:11]([C:10](=[O:15])[CH3:9])[C:12](=[O:14])[CH3:13])=[CH:4][CH:3]=1

Participants

6

Reactant 3

HCID 24436Sodium SulfateHCID 31261AcetylacetoneHCID 784285-Bromothiophene-2-carbaldehyde

Product 1

HCID 19096401HCID 19096401, compound

Reagents, catalysts & solvents 2

HCID 3776IsopropanolSolventHCID 24386Thionyl ChlorideSolvent

Conditions

Temperature
20 °C

Procedure

To a solution containing 5.73 g 5-bromothiophene-2-carboxaldehyde and 5.0 g 2,4-pentanedione in 25 ml of 2-propanol, 2.9 ml thionylchloride was gradually added. The mixture was stirred for 2 h at 20° C. 120 ml of conc. Na2SO4 -solution was then added and the mixture was extracted with ether. The solvent was evaporated in vacuo and the crystalline residue was washed with cold ether. Yield 3.9 g, mp 70°-74° C.

Workup

  1. additionwas gradually added
  2. extractionthe mixture was extracted with ether
  3. customThe solvent was evaporated in vacuo
  4. washthe crystalline residue was washed with cold ether

Sources & evidence

ORD record
ord-67f7c0c03135453aa1d85cef7135743f
Source dataset
uspto-grants-1994_03
Patent number
US05292771

Reaction notes

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