Water → HCID 5076628, compound

HRID 1363426Notes

Reaction equation

HRID 1363426 reaction equation
[OH-:1].[Na+].C(O[CH2:7][C:8]1[CH:13]=[C:12](C)[C:11]([CH2:15][O:16]C(=O)C)=[CH:10][C:9]=1[O:20][CH2:21][CH2:22][CH:23]([CH3:30])[CH2:24][CH2:25][CH2:26][CH:27]([CH3:29])[CH3:28])(=O)C.[OH2:31].[CH3:32]CCCCC>C(O)C>[OH:1][CH2:7][C:8]1[CH:13]=[C:12]([O:31][CH3:32])[C:11]([CH2:15][OH:16])=[CH:10][C:9]=1[O:20][CH2:21][CH2:22][CH:23]([CH3:30])[CH2:24][CH2:25][CH2:26][CH:27]([CH3:29])[CH3:28]

Participants

6

Reactant 4

HCID 962Water2×HCID 8058HexaneHCID 14798Sodium HydroxideHCID 66941269HCID 66941269, compound

Product 1

HCID 5076628HCID 5076628, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
45 °C

Procedure

In a 3 l four-neck flask with condenser and precision glass stirrer, 144.9 g (3.62 mol) of sodium hydroxide were dissolved in 1800 ml of ethanol. After addition of 370 g (0.91 mol) of 2,5-bis(acetoxymethyl)-1-(3,7-dimethyloctyl-oxy)-4-methylbenzene, the mixture was stirred at room temperature for 3 h and at 45° C. for 2.5 h. The mixture was poured onto 2000 ml of water, and the solid which formed was filtered, stirred 3 times with water and filtered again. From the mother liquor, a second fraction was obtained which was likewise stirred 3× with water. The two combined fractions were stirred with hexane at room temperature for 0.5 h, filtered and dried. 183.8 g of white powder were obtained, which were used without further workup and without further characterization directly in the next stage.

Workup

  1. customthe solid which formed
  2. filtrationwas filtered
  3. stirringstirred 3 times with water
  4. filtrationfiltered again
  5. customFrom the mother liquor, a second fraction was obtained which
  6. filtrationfiltered
  7. customdried

Sources & evidence

ORD record
ord-621a0bfb01a143a49d18f92ddbf5bb5b
Source dataset
uspto-grants-2011_02
Patent number
US07884175B2

Reaction notes

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