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1-(1-Acetoxyethyl)-3,5-diacetoxy-benzene → 3,5-Diacetoxy Styrene

HRID 1163268
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HRID 1163268 반응식
C(O[CH:5]([C:7]1[CH:12]=[C:11]([O:13][C:14](=[O:16])[CH3:15])[CH:10]=[C:9]([O:17][C:18](=[O:20])[CH3:19])[CH:8]=1)[CH3:6])(=O)C>C1(C)C=CC=CC=1>[C:14]([O:13][C:11]1[CH:12]=[C:7]([CH:8]=[C:9]([O:17][C:18](=[O:20])[CH3:19])[CH:10]=1)[CH:5]=[CH2:6])(=[O:16])[CH3:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 117375661-(1-Acetoxyethyl)-3,5-diacetoxy-benzene

생성물 1

HCID 113105593,5-Diacetoxy Styrene수율 42.2%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
500 °C

실험 절차

20 g of 1-(1-acetoxyethyl)-3,5-diacetoxy-benzene (71 mmol) were dissolved in 20 ml toluene and placed into a feed vessel connected to a pyrolytic tube filled with Raschig rings. The tube was heated to 500° C. and the neat mixture was immediately added. Conversion of the alcohol was achieved within two minutes. The column was rinsed with toluene. Work-up was conducted by extracting the crude material in toluene twice with 200 ml water. The aqueous solutions were reextracted with toluene, the organic layers were combined, dried over magnesium sulfate and the solvent removed under reduced pressure giving 6.6 g 3,5-diacetoxystyrene (42%).

후처리

  1. customplaced into a feed vessel
  2. customconnected to a pyrolytic tube
  3. additionfilled with Raschig rings
  4. additionthe neat mixture was immediately added
  5. washThe column was rinsed with toluene
  6. extractionby extracting the crude material in toluene twice with 200 ml water
  7. dry with materialdried over magnesium sulfate
  8. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-4384818e26ee41f096313884190b9ad7
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07820848B2

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