Diisopropylethylamine → HCID 71187345, Verbindung

HRID 714401Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 714401
[Br:1][C:2]1[N:6]=[C:5](Cl)[S:4][N:3]=1.Cl.Cl.[CH3:10][O:11][C:12]1[CH:25]=[CH:24][C:15]([CH2:16][CH2:17][N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[CH:14][CH:13]=1.CCN(C(C)C)C(C)C>CCO>[Br:1][C:2]1[N:6]=[C:5]([N:21]2[CH2:20][CH2:19][N:18]([CH2:17][CH2:16][C:15]3[CH:24]=[CH:25][C:12]([O:11][CH3:10])=[CH:13][CH:14]=3)[CH2:23][CH2:22]2)[S:4][N:3]=1

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 27250533-Bromo-5-chloro-1,2,4-thiadiazoleHCID 122357181-(4-Methoxyphenethyl)piperazine dihydrochloride

Produkt 1

HCID 71187345HCID 71187345, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 3-bromo-5-chloro-1,2,4-thiadiazole (300 mg, 1.5 mmol), 1-(4-methoxyphenethyl)piperazine dihydrochloride (485 mg, 1.65 mmol) and DIPEA (641 mg, 867 μl, 4.96 mmol) in EtOH (10 mL) was stirred over night at ambient temperature. The mixture was concentrated in vacuo and the residue was purified by silica column chromatography eluting with a gradient formed from heptane and ethyl acetate to yield after evaporation of the product containing fractions 489 mg (85%) of the title compound as off-white solid. MS (m/e): 383.2 (MH+).

Aufarbeitung

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was purified by silica column chromatography
  3. washeluting with a gradient
  4. customformed from heptane and ethyl acetate
  5. customto yield
  6. customafter evaporation of the product
  7. additioncontaining fractions 489 mg (85%) of the title compound as off-white solid

Quellen und Nachweise

ORD-Eintrag
ord-27dbaa507f8942b98806dacb9d7f3335
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09187440B2

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