Sulfuric Acid → HCID 67127982, compound

HRID 2167753Notes

Reaction equation

HRID 2167753 reaction equation
[CH3:1][O:2][N:3]1[C:8]([CH3:10])([CH3:9])[CH2:7][C:6](=[O:11])[CH2:5][C:4]1([CH3:13])[CH3:12].CC(O)([C:17]#[N:18])C.S(=O)(=O)(O)O.[C:25]([O-:28])(O)=O.[Na+]>C(O)(=O)C>[CH3:1][O:2][N:3]1[C:8]([CH3:9])([CH3:10])[CH2:7][C:6]2([O:11][CH2:17][NH:18][C:25]2=[O:28])[CH2:5][C:4]1([CH3:13])[CH3:12]

Participants

6

Reactant 4

HCID 1118Sulfuric AcidHCID 6406Acetone CyanohydrinHCID 516892Sodium BicarbonateHCID 109761931-Methoxy-2,2,6,6-tetramethylpiperidin-4-one

Product 1

HCID 67127982HCID 67127982, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
70 °C

Procedure

0.61 g of 1-Methoxy-2,2,6,6-tetramethyl-piperidin-4-one and 299 mg acetone cyanhydrine are dissolved in 1.76 g acetic acid and 0.7 g conc. sulfuric acid is added. The reaction mixture is stirred at 70° C. for 18 h. The reaction mixture is added to 40 ml saturated NaHCO3 solution, and extracted with 40 ml ethyl acetate. The organic phase is washed with H2O and subsequently dried over sodium sulfate. The solvent is removed in vacuo to leave 0.61 g of a tan residue. The residue is recrystallized from hexane to yield 0.29 g product. White solid, mp. 130° C.

Workup

  1. extractionextracted with 40 ml ethyl acetate
  2. washThe organic phase is washed with H2O
  3. dry with materialsubsequently dried over sodium sulfate
  4. customThe solvent is removed in vacuo

Sources & evidence

ORD record
ord-7ac05810c621473cabfd03977f4345da
Source dataset
uspto-grants-2015_06
Patent number
US09045480B2

Reaction notes

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