Butyl 3-(p-tert-butylphenoxy)-propionate → 3-p-t-Butyl-phenoxypropanol

HRID 544593

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HRID 544593 반응식
[C:1]([C:5]1[CH:20]=[CH:19][C:8]([O:9][CH2:10][CH2:11][C:12](OCCCC)=[O:13])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-]>CCOCC>[C:1]([C:5]1[CH:20]=[CH:19][C:8]([O:9][CH2:10][CH2:11][CH2:12][OH:13])=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

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온도
-5 °C

실험 절차

This ester 21.0 g was dissolved in 500 ml dry ether and cooled to -5° C. in an ice/acetone bath. To the cold solution was added, cautiously, a slurry of 3.5 g lithium aluminum hydride in 100 ml dry ether. After one hour the excess lithium aluminum hydride was destroyed by the cautious addition of 200 ml ethyl acetate, then 50 ml water. The solution was filtered and the filtrate partitioned between 200 ml ether-200 ml water. The organic layer was removed, dried, and evaporated to a yellow oil which was vacuum distilled (116° C./0.35 mm) over potassium carbonate to a clear colorless oil, 3-p-t-butylphenoxypropanol, 10.1 g (64%).

후처리

  1. additionTo the cold solution was added
  2. customAfter one hour the excess lithium aluminum hydride was destroyed by the cautious addition of 200 ml ethyl acetate
  3. filtrationThe solution was filtered
  4. customthe filtrate partitioned between 200 ml ether-200 ml water
  5. customThe organic layer was removed
  6. customdried
  7. customevaporated to a yellow oil which
  8. distillationdistilled (116° C./0.35 mm) over potassium carbonate to a clear colorless oil, 3-p-t-butylphenoxypropanol, 10.1 g (64%)

출처 및 근거

ORD 기록
ord-ec3529d8b4614a248bfdba0e928d9fb6
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04451474

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