Water → HCID 18959084, compound

HRID 1913988Notes

Reaction equation

HRID 1913988 reaction equation
[C:1]([O:5]O)([CH3:4])([CH3:3])[CH3:2].[OH-:7].[K+].[CH2:9]([CH:11]([CH2:15][CH2:16][CH2:17][CH3:18])[C:12](Cl)=[O:13])[CH3:10].[OH2:19]>>[CH3:18][CH2:17][CH2:16][CH:15]1[O:19][O:7][C:11]1([C:12]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:13])[CH2:9][CH3:10]

Participants

5

Reactant 4

HCID 962Water5×HCID 6410tert-Butyl hydroperoxide2×HCID 14797Potassium Hydroxide2×HCID 791032-Ethylhexanoyl chloride

Product 1

HCID 18959084HCID 18959084, compound

Procedure

The reaction is effected in a reactor arrangement of a first reactor of type E with a downstream reactor of type C. Before the start of the reaction, the first reactor is filled with a solution of 25.8% by weight of tert-butyl hydroperoxide and 16.4% by weight of potassium hydroxide in water. 24.6 kg/h of a solution of 70% by weight of tert-butyl hydroperoxide in water, 24.2 kg/h of a solution of 45% by weight of potassium hydroxide in water, 17.4 kg/h of water and 24.0 kg/h of 2-ethylhexanoyl chloride are then fed to the first reactor. Cooling with cooling water keeps the internal temperature in the first reactor at 35° C. and in the second reactor at 27° C. The organic phase is removed from the reaction mixture withdrawn from the second reactor. The organic phase is washed successively with an 8% by weight solution of sodium hydroxide in water, with a solution of 10% by weight of sodium sulphite in water comprising acetic acid and with a 1% by weight solution of sodium hydrogencarbonate in water, and then dried by stripping in a column with random packing at 33° C. and 35 to 40 mbar. 31.4 kg/h of tert-butyl peroxy-2-ethylhexanoate are obtained (98.5% based on 2-ethylhexanoyl chloride). The space-time yield is 2.53 kg/l·h.

Workup

  1. customThe reaction is effected in a reactor
  2. customBefore the start of the reaction
  3. customat 35° C.
  4. customat 27° C
  5. customThe organic phase is removed from the reaction mixture
  6. customwithdrawn from the second reactor
  7. washThe organic phase is washed successively with an 8% by weight solution of sodium hydroxide in water, with a solution of 10% by weight of sodium sulphite in water
  8. dry with materialwith a 1% by weight solution of sodium hydrogencarbonate in water, and then dried
  9. customby stripping in a column with random packing at 33° C.

Sources & evidence

ORD record
ord-c972e95e239a4c99be44873d1f50f38a
Source dataset
uspto-grants-2013_12
Patent number
US08609883B2

Reaction notes

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