Ethanol → 2-(1-Methyl-3-(pyridin-4-yl)-1H-1,2,4-triazol-5-yl)ethanamine

HRID 1621102Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1621102
[CH3:1][N:2]1[C:6]([CH2:7][CH2:8][N:9]2C(=O)C3C(=CC=CC=3)C2=O)=[N:5][C:4]([C:20]2[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=2)=[N:3]1.CCO>CN>[CH3:1][N:2]1[C:6]([CH2:7][CH2:8][NH2:9])=[N:5][C:4]([C:20]2[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=2)=[N:3]1

Komponenten

4

Edukt 2

HCID 702Ethanol2×HCID 712792712-(2-(1-Methyl-3-(pyridin-4-yl)-1H-1,2,4-triazol-5-yl)ethyl)isoindoline-1,3-dione

Produkt 1

HCID 712792862-(1-Methyl-3-(pyridin-4-yl)-1H-1,2,4-triazol-5-yl)ethanamineAusbeute 74,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6329MethylamineLösungsmittel2×

Versuchsvorschrift

2-(2-(1-Methyl-3-(pyridin-4-yl)-1H-1,2,4-triazol-5-yl)ethyl)isoindoline-1,3-dione (114.9 mg, 345 μmol) was dissolved in methylamine solution in EtOH (3.07 mL, 22.5 mmol) and stirred at RT for 1 h. The reaction mixture was evaporated to give light brown solid. The solid was again dissolved in methylamine solution in EtOH (3.07 mL, 22.5 mmol) and the mixture was heated to 50° C. and stirred for 3 h. All volatiles were removed in vacuo and the residue was suspended in dichloromethane (1.5 mL) and filtered. The filtrate was evaporated to give the product as light yellow solid (81.3 mg (80% purity), 256 μmol, 74.2%) which was used without purification for the next step. MS: M=204.2 (M+H)+

Aufarbeitung

  1. customThe reaction mixture was evaporated
  2. customto give light brown solid
  3. temperaturethe mixture was heated to 50° C.
  4. stirringstirred for 3 h
  5. customAll volatiles were removed in vacuo
  6. filtrationfiltered
  7. customThe filtrate was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-2aa591603db545b990db7cbae8398156
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08772510B2

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