Sodium Sulfate → HCID 53770654, compound

HRID 893363Notes

Reaction equation

HRID 893363 reaction equation
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][C:7]([CH3:15])([CH3:14])[CH2:8][C:9](OCC)=[O:10].[H-].[Al+3].[Li+].[H-].[H-].[H-].S([O-])([O-])(=O)=O.[Na+].[Na+]>CCOCC>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][C:7]([CH3:15])([CH3:14])[CH2:8][CH2:9][OH:10]

Participants

5

Reactant 3

HCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydrideHCID 53973528HCID 53973528, compound

Product 1

HCID 53770654HCID 53770654, compoundYield 117.3%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

86.7 g of ethyl 4-(dioxolan-2-yl)-3,3-dimethylbutanoate, prepared above, are dissolved in 720 ml of ether. This solution is added dropwise at 10° C. to a suspension of 9 g of lithium aluminum hydride in 700 ml of ether. When the addition is complete, the mixture is stirred for 3 hours at room temperature and then cooled to 10° C. A saturated solution of sodium sulfate is added dropwise at this temperature until a granular precipitate is obtained, which is filtered off. The ether filtrate is evaporated to dryness at a temperature below 30° C. to give 81.9 g of 4-(dioxolan-2-yl)-3,3-dimethylbutanol in the form of an oil, which is used as such for the next step.

Workup

  1. additionWhen the addition
  2. temperaturecooled to 10° C
  3. customis obtained
  4. filtrationwhich is filtered off
  5. customThe ether filtrate is evaporated to dryness at a temperature below 30° C.

Sources & evidence

ORD record
ord-a9beab5ced3142929da4042f8bfbb484
Source dataset
uspto-grants-1992_06
Patent number
US05124336

Reaction notes

Loading…