Hydrochloric Acid → tert-Butyl peroxy-3,5,5-trimethylhexanoate

HRID 909414노트

반응식

HRID 909414 반응식
[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].Cl>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]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6410tert-Butyl hydroperoxide2회HCID 14797Potassium Hydroxide2회HCID 1619293,5,5-Trimethylhexanoyl chloride

생성물 1

HCID 114465tert-Butyl peroxy-3,5,5-trimethylhexanoate수율 98.2%

시약·촉매·용매 1

HCID 962Water용매5회

실험 절차

Before the start of the reaction, the loop reactor is filled with a solution of 25.7% by weight of tert-butyl hydroperoxide and 15.0% by weight of potassium hydroxide in water. Initially 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 loop reactor. Cooling with cooling water keeps the internal temperature at 25° C. in the loop reactor and in the stirred cell reactor. The partial neutralization is effected with 27.6 kg/h of 4% by weight hydrochloric acid at a temperature of 15° C. The organic phase is extracted with 23.6 kg/h of a 20% by weight aqueous solution of potassium hydroxide. This affords 26.2 kg/h of aqueous extract comprising 9.6% by weight of tert-butyl hydroperoxide and 18.0% by weight of potassium hydroxide, which are feeded into the loop reactor. From the time at which aqueous extract is recycled into the loop reactor, the metered addition of the feedstocks is changed to 16.6 kg/h of a solution of 70% by weight of tert-butyl hydroperoxide in water, 7.8 kg/h of a solution of 45% by weight of potassium hydroxide in water and 4.8 kg/h of water. After the extraction, the organic phase is washed with 33.8 kg/h of a solution of 3% by weight of sodium sulphite and 1% by weight of sulphuric acid, and dried by stripping at 34° C. and 47 mbar. 24.6 kg/h of tert-butyl peroxy-3,5,5-trimethylhexanoate with a purity of 99.9% are obtained (98.2% yield based on 3,5,5-trimethylhexanoyl chloride).

후처리

  1. customBefore the start of the reaction
  2. customat 25° C.
  3. extractionThe organic phase is extracted with 23.6 kg/h of a 20% by weight aqueous solution of potassium hydroxide
  4. extractionThis affords 26.2 kg/h of aqueous extract
  5. extractionFrom the time at which aqueous extract
  6. additionthe metered addition of the feedstocks
  7. extractionAfter the extraction
  8. washthe organic phase is washed with 33.8 kg/h of a solution of 3% by weight of sodium sulphite and 1% by weight of sulphuric acid
  9. customdried
  10. customby stripping at 34° C.

출처 및 근거

ORD 기록
ord-50e528ad68084a3d8e1d10ffc54f3236
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017801B2

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