Sulfuric Acid → HCID 69971292, compound

HRID 2185916Notes

Reaction equation

HRID 2185916 reaction equation
[Mg].[C:2](OCC)(=O)CC(OCC)=O.Cl[C:14]([C:16]1[O:17][C:18]2[C:27]([CH:28]=[CH:29][CH3:30])=[CH:26][CH:25]=[CH:24][C:19]=2[C:20](=[O:23])[C:21]=1[CH3:22])=[O:15].S(=O)(=O)(O)O>C(O)C.C1(C)C=CC=CC=1.C(Cl)(Cl)Cl.O.C(Cl)(Cl)(Cl)Cl>[C:14]([C:16]1[O:17][C:18]2[C:27]([CH:28]=[CH:29][CH3:30])=[CH:26][CH:25]=[CH:24][C:19]=2[C:20](=[O:23])[C:21]=1[CH3:22])(=[O:15])[CH3:2]

Participants

10

Reactant 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 5462224MagnesiumHCID 88079847HCID 88079847, compound

Product 1

HCID 69971292HCID 69971292, compound

Reagents, catalysts & solvents 5

HCID 702EthanolSolventHCID 962WaterSolventHCID 1140TolueneSolventHCID 5943Carbon TetrachlorideSolventHCID 6212ChloroformSolvent

Procedure

0.051 g of magnesium turnings were suspended in 10 mL of anhydrous ethanol. 0.3 mL of carbon tetrachloride and 0.32 mL of diethyl malonate were added and the resulting mixture was stirred at room temperature (with spontaneous heating) for 1 hour, then at 60° C. for 2 hours and cooled to room temperature. A solution of 0.42 g of Compound 2A in 15 mL of toluene and chloroform (5 mL) was added dropwise and the resulting mixture was stirred at room temperature for 6 hours. After overnight resting, 0.12 mL of 98% sulphuric acid and 3 mL of water were added; the precipitated inorganic salts were filtered off and the filtrate was evaporated under vacuum to dryness.

Workup

  1. temperature(with spontaneous heating) for 1 hour
  2. temperaturecooled to room temperature
  3. stirringthe resulting mixture was stirred at room temperature for 6 hours
  4. waitAfter overnight resting
  5. filtrationthe precipitated inorganic salts were filtered off
  6. customthe filtrate was evaporated under vacuum to dryness

Sources & evidence

ORD record
ord-115c859b310a43ad9e212d70bade583f
Source dataset
uspto-grants-2002_06
Patent number
US06403594B1

Reaction notes

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