Sulfuric Acid → HCID 86100631, compound

HRID 878849Notes

Reaction equation

HRID 878849 reaction equation
S(=O)(=O)(O)[OH:2].[CH:6]([C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[C:10]([CH3:16])[CH:9]=1)=[O:7]>>[CH:6]([C:8]1[CH:15]=[CH:14][C:11]([C:12]([NH2:13])=[O:2])=[C:10]([CH3:16])[CH:9]=1)=[O:7]

Participants

3

Reactant 2

HCID 1118Sulfuric AcidHCID 45083566Benzonitrile, 4-formyl-2-methyl- (9CI)

Product 1

HCID 86100631HCID 86100631, compound

Procedure

In 0.40 g of 4-formyl-2-methylbenzonitrile, 7 mL of concentrated sulfuric acid was added, and stirred at room temperature for 4.5 days. After the completion of the reaction, the reaction mixture was poured in 20 mL of ice water, extracted with ethyl acetate (15 mL×2). The combined organic phases were washed with water, and dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was washed with 5 mL of diisopropyl ether to obtain 0.26 g of the aimed product as white crystal.

Workup

  1. customAfter the completion of the reaction
  2. extractionextracted with ethyl acetate (15 mL×2)
  3. washThe combined organic phases were washed with water
  4. dry with materialdried over saturated sodium chloride aqueous solution
  5. distillationanhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure
  6. washThe residue was washed with 5 mL of diisopropyl ether

Sources & evidence

ORD record
ord-e1aa3a44836d4019aa56580b76207850
Source dataset
uspto-grants-2015_03
Patent number
US08987464B2

Reaction notes

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