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Acrylic Acid → 6-Hydroxy-5,7,8-trimethyl-chroman-2-one

HRID 2102984
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HRID 2102984 반응식
[CH3:1][C:2]1[C:3]([OH:11])=[C:4]([CH3:10])[C:5]([CH3:9])=[C:6]([CH:8]=1)[OH:7].[C:12](O)(=[O:15])[CH:13]=[CH2:14]>CS(O)(=O)=O>[OH:11][C:3]1[C:2]([CH3:1])=[C:8]2[C:6](=[C:5]([CH3:9])[C:4]=1[CH3:10])[O:7][C:12](=[O:15])[CH2:13][CH2:14]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6581Acrylic AcidHCID 12785Trimethylhydroquinone

생성물 1

HCID 2973756-Hydroxy-5,7,8-trimethyl-chroman-2-one수율 43%

시약·촉매·용매 1

HCID 6395Methanesulfonic Acid용매

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온도
100 °C

실험 절차

To a mixture of trimethyl-hydroquinone (3.04 g) and acrylic acid (1.44 g) was added methyl-sulfonic acid (30 mL). The mixture was heated slowly up to 100° C. under nitrogen. The reaction mixture was stirred at 100° C. for 1 hour. The solution was poured into ice, and extracted with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate water solution, water and brine. Evaporation and chromatography (silica gel, hexane-ethyl acetate 10% to 25%) gave 1.77 g of 6-hydroxy-5,7,8-trimethyl-chroman-2-one.

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후처리

  1. additionThe solution was poured into ice
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated sodium bicarbonate water solution, water and brine
  4. customEvaporation and chromatography (silica gel, hexane-ethyl acetate 10% to 25%)

출처 및 근거

ORD 기록
ord-50e884a726b04268a29f0971abcc353d
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576094B2

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