Water → HCID 67099655, compound

HRID 2078037Notes

Reaction equation

HRID 2078037 reaction equation
OS(O)(=O)=O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:28])([CH3:27])[C:14]([CH:16]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:17](OCC)=[O:18])=[O:15])=[CH:9][CH:8]=1.O>CCCCCCC>[Cl:6][C:7]1[CH:12]=[C:11]2[C:10](=[CH:9][CH:8]=1)[C:13]([CH3:27])([CH3:28])[C:14](=[O:15])[C:16]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[C:17]2[OH:18]

Participants

5

Reactant 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 67099102HCID 67099102, compound

Product 1

HCID 67099655HCID 67099655, compoundYield 79.9%

Reagents, catalysts & solvents 1

HCID 8900HeptaneSolvent

Procedure

Concentrated H2SO4 (5.0 mL, 18.0M) was cooled to −4° C. and treated with diethyl 2-(2-(4-chlorophenyl)-2-methylpropanoyl)malonate (1.00 g, 2.93 mmol). The resulting green solution was warmed to room temperature and allowed to stir for 1 hour. The solution was then poured into a 0° C. chilled mixture of water (10 mL) and heptane (5 mL). The resulting precipitate was collected by vacuum filtration, washed with cold water (10 mL) and heptane (1 mL). The product was dried at 40° C. overnight under vacuum to give 0.69 g of the title compound. MS m/e=295.2 (M+H)+.

Workup

  1. additionThe solution was then poured into a 0° C.
  2. temperaturechilled
  3. filtrationThe resulting precipitate was collected by vacuum filtration
  4. washwashed with cold water (10 mL) and heptane (1 mL)
  5. customThe product was dried at 40° C. overnight under vacuum

Sources & evidence

ORD record
ord-7ae9920aa1b14d5a8404df65b61976ae
Source dataset
uspto-grants-2011_04
Patent number
US07928139B2

Reaction notes

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