Water → HCID 548881, compound

HRID 1731484Notes

Reaction equation

HRID 1731484 reaction equation
[C:1]1(=[O:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.O.[OH-].[Na+].[CH:11](=O)[CH:12]([CH3:14])[CH3:13]>[Cl-].[Na+].O>[CH:11](=[C:2]1[CH2:3][CH2:4][CH2:5][CH2:6][C:1]1=[O:7])[CH:12]([CH3:14])[CH3:13]

Participants

6

Reactant 4

HCID 962WaterHCID 6561IsobutyraldehydeHCID 7967CyclohexanoneHCID 14798Sodium Hydroxide

Product 1

HCID 548881HCID 548881, compoundYield 40%

Reagents, catalysts & solvents 1

HCID 57417360Sodium chloride; waterSolvent

Procedure

Into a 8 liter reaction vessel are placed 3400 grams cyclohexanone, 250 grams of water and 80 grams of sodium hydroxide. Over a period of one hour while maintaining the reaction mass at 50°-75° C., 1400 grams (19.4 moles) of isobutyraldehyde is added to the reaction mass. The reaction mass is stirred for a period of one hour. At the end of the one hour period, an equal volume of brine is added to the reaction mass. The organic phase is separated from the aqueous phase and the organic phase is washed with two volumes of brine. 500 ml Toluene is added to the organic phase and the water is azeotroped from the reaction mass. The reaction mass is then distilled yielding 1180 grams of product, the distillation taking place on a 2" splash column yielding the following fractions:

Workup

  1. customInto a 8 liter reaction vessel
  2. temperatureOver a period of one hour while maintaining the reaction mass at 50°-75° C.
  3. customThe organic phase is separated from the aqueous phase
  4. washthe organic phase is washed with two volumes of brine
  5. addition500 ml Toluene is added to the organic phase
  6. customthe water is azeotroped from the reaction mass
  7. distillationThe reaction mass is then distilled

Sources & evidence

ORD record
ord-68a88c6853964f4b80f641081bb69ec0
Source dataset
uspto-grants-1986_11
Patent number
US04622172

Reaction notes

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