StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

1,2-Dichloroethane → HCID 68703969, Verbindung

HRID 1619223
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1619223
C(O[C:6]([N:8]1[CH:13]2[CH2:14][CH2:15][CH:9]1[CH2:10][N:11]([C:16]1[N:21]=[CH:20][CH:19]=[CH:18][N:17]=1)[CH2:12]2)=[O:7])(C)(C)C.FC(F)(F)C1[CH:25]=[C:26]([C:30]2[CH:35]=[CH:34][C:33](C(O)=O)=[CH:32][CH:31]=2)[CH:27]=CC=1.[CH2:41](Cl)[CH2:42]Cl.[CH:45]1[CH:46]=CC2N(O)N=N[C:49]=2[CH:50]=1.Cl.O1CCOC[CH2:57]1>O.CCOC(C)=O>[C:26]([C:30]1[CH:31]=[C:32]([C:42]2[CH:41]=[CH:49][C:50]([C:6]([N:8]3[CH:9]4[CH2:15][CH2:14][CH:13]3[CH2:12][N:11]([C:16]3[N:17]=[CH:18][CH:19]=[CH:20][N:21]=3)[CH2:10]4)=[O:7])=[CH:45][CH:46]=2)[CH:33]=[CH:34][CH:35]=1)([CH3:25])([CH3:27])[CH3:57]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 27827173'-(Trifluoromethyl)[1,1'-biphenyl]-4-carboxylic acidHCID 204431481,4-Dioxane hydrochlorideHCID 68700570HCID 68700570, Verbindung

Produkt 1

HCID 68703969HCID 68703969, Verbindung
Ausbeute 32 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A solution of 3-pyrimidin-2-yl-3,8-diaza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (64 mg, 0.22 mmol) in HCl/dioxane was stirred for 5 hours at room temperature. The resulting solution was concentrated, and the residue was dissolved in CH2Cl2 (5 mL) and added to a solution of 3′-trifluoromethyl-biphenyl-4-carboxylic acid (117 mg, 0.44 mmol), EDC (85 mg, 0.44 mmol), HOBt (60 mg, 0.44 mol) and TEA (0.1 mL, 0.71 mmol). After stirring overnight, the mixture was treated with EtOAc (50 mL) and water (15 mL). The organic phase was washed with brine (5 mL), dried (MgSO4), filtered, and concentrated under reduced pressure to furnish the crude product. This material was purified by column chromatography (30% EtOAc/hexanes) to give the title compound 14.2 mg, (32%) as a white solid: 1H NMR (DMSO): δ 8.35 (d, J=12 Hz, 2H), 7.79-7.76 (m, 3H), 7.68 (dt, J=20, 3 Hz, 1H), 7.63 (d, J=21 Hz, 2H), 7.52-7.43 (m, 2H), 6.62 (t, J=12 Hz, 1H), 4.77 (bs, 1H), 4.41 (d, J=64 Hz, 2H), 4.17 (bs, 1H), 3.14 (bs, 2H), 2.48 (qt, J=5 Hz, 1H), 1.86 (t, J=9 Hz, 2H), 1.60 (d, J=24 Hz, 1H); MS (M+1)=439.

Aufarbeitung

  1. concentrationThe resulting solution was concentrated
  2. dissolutionthe residue was dissolved in CH2Cl2 (5 mL)
  3. washThe organic phase was washed with brine (5 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customto furnish the crude product
  8. customThis material was purified by column chromatography (30% EtOAc/hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-a90f22ee11f645bab735ec4b6c5d2cd0
Quelldatensatz
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08772291B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion