tert-Butyl hydroperoxide → tert-Butyl peroxy-3,5,5-trimethylhexanoate

HRID 1913991ノート

反応式

HRID 1913991 の反応式
[C:1]([O:5][OH:6])([CH3:4])([CH3:3])[CH3:2].[OH-].[K+].[CH3:9][CH:10]([CH2:15][C:16]([CH3:19])([CH3:18])[CH3:17])[CH2:11][C:12](Cl)=[O:13]>O>[CH3:9][CH:10]([CH2:15][C:16]([CH3:19])([CH3:18])[CH3:17])[CH2:11][C:12]([O:6][O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:13]

参加物

5

反応物 3

HCID 6410tert-Butyl hydroperoxide2 回HCID 14797Potassium Hydroxide2 回HCID 1619293,5,5-Trimethylhexanoyl chloride

生成物 1

HCID 114465tert-Butyl peroxy-3,5,5-trimethylhexanoate

試薬・触媒・溶媒 1

HCID 962Water溶媒5 回

実験手順

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 25.6% by weight of tert-butyl hydroperoxide and 15.0% by weight of potassium hydroxide in water. 20.2 kg/h of a solution of 70% by weight of tert-butyl hydroperoxide in water, 18.2 kg/h of a solution of 45% by weight of potassium hydroxide in water, 16.2 kg/h of water and 19.2 kg/h of 3,5,5-trimethylhexanoyl chloride are then fed to the first reactor. Cooling with cooling water keeps the internal temperature in the first reactor at 25° C. and in the second reactor at 25° C. The organic phase is removed from the reaction mixture withdrawn from the second reactor.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 hydrogen-carbonate in water, and then dried by stripping in a packed column at 34° C. and 47 mbar. 24.6 kg/h of tert-butyl peroxy-3,5,5-trimethylhexanoate are obtained (98.2% based on 3,5,5-trimethylhexanoyl chloride). The space-time yield is 1.98 kg/l·h.

後処理

  1. customThe reaction is effected in a reactor
  2. customBefore the start of the reaction
  3. customat 25° C.
  4. customat 25° 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 hydrogen-carbonate in water, and then dried
  9. customby stripping in a packed column at 34° C.

出典と根拠

ORDレコード
ord-cfb1d502e88e4228b1519d9f7df0927c
出典データセット
uspto-grants-2013_12
特許番号
US08609883B2

反応ノート

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