Potassium Hydroxide → 2-[4-(8-Hydroxy-2,2,4,4-tetramethyl-chroman-6-ylethynyl)-phenyl]-2-methyl-propionic acid

HRID 1869861Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1869861
C[O:2][C:3](=[O:30])[C:4]([C:7]1[CH:12]=[CH:11][C:10]([C:13]#[C:14][C:15]2[CH:16]=[C:17]3[C:22](=[C:23]([OH:25])[CH:24]=2)[O:21][C:20]([CH3:27])([CH3:26])[CH2:19][C:18]3([CH3:29])[CH3:28])=[CH:9][CH:8]=1)([CH3:6])[CH3:5].[OH-].[K+]>CO.O1CCCC1>[OH:25][C:23]1[CH:24]=[C:15]([C:14]#[C:13][C:10]2[CH:11]=[CH:12][C:7]([C:4]([CH3:6])([CH3:5])[C:3]([OH:30])=[O:2])=[CH:8][CH:9]=2)[CH:16]=[C:17]2[C:22]=1[O:21][C:20]([CH3:27])([CH3:26])[CH2:19][C:18]2([CH3:29])[CH3:28]

Komponenten

5

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A solution of 2-[4-(8-hydroxy-2,2,4,4-tetramethyl-chroman-6-ylethynyl)-phenyl]-2-methyl-propionic acid methyl ester (Intermediate 23, 0.035 g, 0.087 mmol) in methanol (2 mL) and tetrahydrofuran (1 mL) was treated with a 1M solution of potassium hydroxide (2 mL, 4 mmol) and the resulting reaction mixture was stirred at 80° C. for 2 h. The volatiles were evaporated in vacuo to a residue that was neutralized with saturated aqueous ammonium chloride solution and extracted with ethyl acetate. The organic phase was washed with water and brine, and dried over anhydrous magnesium sulfate, filtered and evaporated in vacuo to afford the title product as a yellow solid (0.034 g, 100%).

Aufarbeitung

  1. customthe resulting reaction mixture
  2. customThe volatiles were evaporated in vacuo to a residue that
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was washed with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e01de9489e624fe09892bb68dc491ed8
Quelldatensatz
uspto-grants-2009_12
Patentnummer
US07638648B2

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