1,4-Dioxane hydrochloride → 2-[(4-{2-[(5-Bromopyridin-2-yl)(heptyl)amino]ethyl}-1,3-thiazol-2-yl)thio]-2-methylpropionic acid hydrochloride

HRID 914426Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 914426
C([O:5][C:6](=[O:33])[C:7]([S:10][C:11]1[S:12][CH:13]=[C:14]([CH2:16][CH2:17][N:18]([C:26]2[CH:31]=[CH:30][C:29]([Br:32])=[CH:28][N:27]=2)[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[N:15]=1)([CH3:9])[CH3:8])(C)(C)C.[ClH:34].O1CCOCC1>O1CCOCC1>[ClH:34].[Br:32][C:29]1[CH:30]=[CH:31][C:26]([N:18]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:17][CH2:16][C:14]2[N:15]=[C:11]([S:10][C:7]([CH3:8])([CH3:9])[C:6]([OH:33])=[O:5])[S:12][CH:13]=2)=[N:27][CH:28]=1

Komponenten

4

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 597594422-[(4-{2-[(5-Bromopyridin-2-yl)(heptyl)amino]ethyl}-1,3-thiazol-2-yl)thio]-2-methylpropionic acid tert-butyl ester

Produkt 1

HCID 673983692-[(4-{2-[(5-Bromopyridin-2-yl)(heptyl)amino]ethyl}-1,3-thiazol-2-yl)thio]-2-methylpropionic acid hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

2-[(4-{2-[(5-Bromopyridin-2-yl)(heptyl)amino]ethyl}-1,3-thiazol-2-yl)thio]-2-methylpropionic acid tert-butyl ester (1.72 g) synthesized in Example 293-1 was dissolved in dioxane (5 mL), 4 mol/L hydrochloric acid-dioxane (25 mL) was added, and the mixture was stirred at room temperature for 12 hr. The reaction mixture was concentrated under reduced pressure, azeotroped with diethyl ether, and the precipitated solid was collected by filtration to give the title compound (1.0 g) as a white solid.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customazeotroped with diethyl ether
  3. filtrationthe precipitated solid was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-ee304994f2ed4b4385f2ac823cde31d9
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08026370B2

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