Diisopropylethylamine → 1,1-Dimethylethyl 3-methyl-4-[(1-phenyl-1H-1,2,4-triazol-3-yl)carbonyl]-1-piperazinecarboxylate

HRID 334078Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 334078
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH:10]([CH3:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CCN(C(C)C)C(C)C.[C:24]1([N:30]2[CH:34]=[N:33][C:32]([C:35](Cl)=[O:36])=[N:31]2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C(Cl)Cl>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:35]([C:32]2[N:33]=[CH:34][N:30]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[N:31]=2)=[O:36])[CH:10]([CH3:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 2756810tert-Butyl 3-methylpiperazine-1-carboxylateHCID 866882991-Phenyl-1H-1,2,4-triazole-3-carbonyl chloride

Produkt 1

HCID 866883001,1-Dimethylethyl 3-methyl-4-[(1-phenyl-1H-1,2,4-triazol-3-yl)carbonyl]-1-piperazinecarboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a mixture of 2.19 g (10.5 mmol) 3-methyl-piperazine-1-carboxylic acid tert-butyl ester and 2.50 mL (14.6 mmol) DIPEA in 15 mL DCM was added a solution of 2.18 g (10.5 mmol) 1-phenyl-1H-[1,2,4]-triazole-3-carbonyl chloride in 15 mL DCM. The reaction mixture was stirred at RT for 3 days, then washed with water. The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo.

Aufarbeitung

  1. washwashed with water
  2. dry with materialThe combined organic phases were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-9aacb79db5a94d16a744a7e593cf5896
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08883789B2

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