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Dimethylformamide → 3,4-dicyclopropyl-5-(4-pentylbicyclo[2.2.2]oct-1-yl)-4H-1,2,4-triazole

HRID 913049
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 913049
[CH:1]1([NH:4][C:5]([CH:7]2[CH2:9][CH2:8]2)=O)[CH2:3][CH2:2]1.O(C)S(C(F)(F)F)(=O)=O.[CH2:19]([C:24]12[CH2:31][CH2:30][C:27]([C:32]([NH:34][NH2:35])=O)([CH2:28][CH2:29]1)[CH2:26][CH2:25]2)[CH2:20][CH2:21][CH2:22][CH3:23].CN(C=O)C.C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH:7]1([C:5]2[N:4]([CH:1]3[CH2:3][CH2:2]3)[C:32]([C:27]34[CH2:28][CH2:29][C:24]([CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])([CH2:31][CH2:30]3)[CH2:25][CH2:26]4)=[N:34][N:35]=2)[CH2:9][CH2:8]1
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Komponenten

7

Edukt 5

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 9526Methyl triflateHCID 351205Cyclopropanecarboxylic acid cyclopropylamideHCID 225916944-Pentylbicyclo[2.2.2]octane-1-carbohydrazide

Produkt 1

HCID 111748243,4-dicyclopropyl-5-(4-pentylbicyclo[2.2.2]oct-1-yl)-4H-1,2,4-triazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

To a solution of N-cyclopropylcyclopropanecarboxamide (2-A) (26 mg, 0.210 mmol) in 0.50 ml toluene was added methyl triflate (1.45 mg, 1 eq) and the reaction was heated at 100° C. for 5-7 min until all of the amide went into solution. To this crude solution was added 0.740 mL of a 0.3 M solution of 4-pentylbicyclo[2.2.2]octane-1-carbohydrazide in DMF (1.1 eq, crude, prepared as described in Step A of Example 1) followed by triethylamine (0.059 mL, 2 eq) and the mixture was heated at 130° C. for 4 h. After this time the solvent was removed under reduced pressure, and the residue was chromatographed on C-18 reverse phase (gradient 90% water to 100% acetonitrile, 0.1% TPA). The fractions containing the compound were determined by LCMS, added to 200 mL of methylene chloride, and extracted with saturated aqueous sodium bicarbonate. The organic layer was dried over magnesium sulfate and evaporated under diminished. The residue was lyophilized from benzene to afford 3,4-dicyclopropyl-5-(4-pentylbicyclo[2.2.2]oct-1-yl)-4H-1,2,4-triazole (2-B); MS (ESI+)=328.3 (M+1).

Aufarbeitung

  1. customAfter this time the solvent was removed under reduced pressure
  2. customthe residue was chromatographed on C-18 reverse phase (gradient 90% water to 100% acetonitrile, 0.1% TPA)
  3. additionThe fractions containing the compound
  4. additionadded to 200 mL of methylene chloride
  5. extractionextracted with saturated aqueous sodium bicarbonate
  6. dry with materialThe organic layer was dried over magnesium sulfate
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-ccf9927c7ff24b85a97bb67107f64af1
Quelldatensatz
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08026264B2

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