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

HRID 2102984
ノート
印刷プレビュー

反応式

HRID 2102984 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6581Acrylic AcidHCID 12785Trimethylhydroquinone

生成物 1

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

試薬・触媒・溶媒 1

HCID 6395Methanesulfonic Acid溶媒

反応条件

温度
100 °C

実験手順

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.

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  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%)

出典と根拠

ORDレコード
ord-50e884a726b04268a29f0971abcc353d
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07576094B2

反応ノート

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