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Hydroxyphenylacetic acid → Pterostilbene

HRID 59013
ノート
印刷プレビュー

反応式

HRID 59013 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([O:11][CH3:12])[CH:10]=1)[CH:6]=O.[OH:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][C:21]([OH:23])=[O:22])=[CH:16][CH:15]=1.Cl>C(OC(=O)C)(=O)C.C(N(CC)CC)C.C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[C:5](/[CH:6]=[CH:20]/[C:17]2[CH:16]=[CH:15][C:14]([OH:13])=[CH:19][CH:18]=2)[CH:4]=1.[CH3:1][O:2][C:3]1[CH:4]=[C:5](/[CH:6]=[C:20](/[C:17]2[CH:18]=[CH:19][C:14]([OH:13])=[CH:15][CH:16]=2)\[C:21]([OH:23])=[O:22])[CH:8]=[C:9]([O:11][CH3:12])[CH:10]=1
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

8

反応物 3

HCID 127Hydroxyphenylacetic acidHCID 313Hydrochloric AcidHCID 817473,5-Dimethoxybenzaldehyde

生成物 2

HCID 5281727PterostilbeneHCID 5386532Z-3-(3,5-Dimethoxyphenyl)-2-(4-hydroxyphenyl)-acrylic acid

試薬・触媒・溶媒 3

HCID 6212Chloroform溶媒
HCID 7918
Acetic Anhydride
溶媒
HCID 8471Triethylamine溶媒

反応条件

温度
150 °C

実験手順

Pterostilbene was synthesized as previously described (Joseph et al., supra). Briefly, pterostilbene was synthesized by condensation of 3,5-dimethoxybenzaldehyde and 4-hydroxyphenylacetic acid in acetic anhydride and triethylamine. The reaction mixture was heated (150° C.) under an atmosphere of nitrogen and continuously stirred. After 20 h, the reaction was stopped and cooled to room temperature, and concentrated hydrochloric acid (5 mL) was added. A precipitate formed, and this was dissolved in 50 mL of chloroform and then extracted with 10% aqueous sodium hydroxide. The aqueous extract was acidified to pH 1 with concentrated hydrochloric acid and stirred for at least 6 h, resulting in the precipitation of the intermediate product, α-[(3,5-dimethoxyphenyl)methylene]-4-hydroxy-(αZ)-benzeneacetic acid. This intermediate product was heated with 1.0 g of copper in 10 mL of quinoline (200° C., 6 h, under nitrogen). The reaction mixture was cooled to room temperature and filtered. To the filtrate was added 5 N hydrochloric acid (25 mL), which Was stirred for 1 h and then extracted with chloroform. The chloroform extract containing impure pterostilbene was purified by flash chromatography on a Horizon HPFC system (Biotage, Inc., Charlottesville, Va.), using a silica gel column and the solvent system ethyl acetate:hexane (linear gradient from 15:85 to 100% ethyl acetate). Fractions containing pure pterostilbene were combined and concentrated in vacuum. Pterostilbene was recrystallized in hexane, and its structure was confirmed from its spectroscopic data (UV, mass spectrometry, and nuclear magnetic resonance spectroscopy) (FIG. 1).

後処理

  1. customPterostilbene was synthesized
  2. temperaturecooled to room temperature
  3. customA precipitate formed
  4. extractionextracted with 10% aqueous sodium hydroxide
  5. extractionThe aqueous extract
  6. stirringstirred for at least 6 h

出典と根拠

ORDレコード
ord-9b59ebfc5a434621b607ba183ede0c95
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09439875B2

反応ノート

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