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Potassium Hydroxide → 1,1-Dimethylethyl 4-ethenylphenyl carbonate

HRID 1657216
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HRID 1657216 반응식
C(OC1[CH:12]=[CH:11][C:8]([CH:9]=[CH2:10])=[CH:7][CH:6]=1)(=O)C.[OH-].[K+].C(O[C:20]([O:22][C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])=O)(C)(C)C>[OH-].[K+].C(O)C>[C:26]([O:25][C:23]([O:22][C:20]1[CH:10]=[CH:9][C:8]([CH:11]=[CH2:12])=[CH:7][CH:6]=1)=[O:24])([CH3:27])([CH3:28])[CH3:29]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 14797Potassium HydroxideHCID 758214-Ethenylphenyl acetateHCID 90495Di-tert-butyl dicarbonate

생성물 1

HCID 934851,1-Dimethylethyl 4-ethenylphenyl carbonate수율 64%

시약·촉매·용매 2

HCID 14797Potassium Hydroxide촉매HCID 702Ethanol
용매

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온도
28 °C

실험 절차

A solution comprising 0.49 grams potassium hydroxide, 40 grams of 4-acetoxystyrene, and 100 grams of absolute ethanol was refluxed for 4 hours. The reaction solution was cooled to 28° C. and 13 grams of potassium hydroxide pellets were added over a period of 10 minutes. After an additional 30 minutes of reaction, 64 grams di-tertiary-butyl-dicarbonate was charged portionwise over 20 minutes and the reaction was stirred for an additional hour at 28° C. After aqueous washing, the reaction product was extracted with ethyl acetate. The ethyl acetate was stripped from the extraction mixture on a rotary evaporator and the residual oil was charged with 0.07 grams phenothiazine. Distillation at 0.1 mm Hg gave 34.2 grams (64%) 4-tertiary-butoxycarbonyloxystyrene.

후처리

  1. temperaturewas refluxed for 4 hours
  2. additionwas charged portionwise over 20 minutes
  3. extractionAfter aqueous washing, the reaction product was extracted with ethyl acetate
  4. customThe ethyl acetate was stripped from the extraction mixture on a rotary evaporator
  5. additionthe residual oil was charged with 0.07 grams phenothiazine
  6. distillationDistillation at 0.1 mm Hg

출처 및 근거

ORD 기록
ord-2a80e22c2f2e417db18bb9ccc62dd37f
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05256809

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