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Triphenylphosphine → 3-(7-cyano-1,2,3,4-tetrahydro-naphthalen-1-yl)-3H-imidazole-4-carboxylic acid isopropyl ester

HRID 2089473
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Reaktionsgleichung

Reaktionsgleichung von HRID 2089473
[C:1]([C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][CH2:9][CH:10]2O)=[CH:5][CH:4]=1)#[N:2].[NH:14]1[CH:18]=[C:17]([C:19]([O:21][CH:22]([CH3:24])[CH3:23])=[O:20])[N:16]=[CH:15]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>C1COCC1.C(OCC)(=O)C>[CH:22]([O:21][C:19]([C:17]1[N:16]([CH:10]2[C:11]3[C:6](=[CH:5][CH:4]=[C:3]([C:1]#[N:2])[CH:12]=3)[CH2:7][CH2:8][CH2:9]2)[CH:15]=[N:14][CH:18]=1)=[O:20])([CH3:24])[CH3:23]
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Komponenten

7

Edukt 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 572782727-Cyano-1,2,3,4-tetrahydro-naphthalen-1-olHCID 178459416HCID 178459416, Verbindung

Produkt 1

HCID 591993833-(7-cyano-1,2,3,4-tetrahydro-naphthalen-1-yl)-3H-imidazole-4-carboxylic acid isopropyl ester

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a suspension of 7-cyano-1,2,3,4-tetrahydro-naphthalen-1-ol (0.298 g, 1.72 mmol) and isopropyl 4-imidazolecarboxylate (0.185 g, 1.204 mmol), which can be prepared as described in Example 1, in THF (10 mL) at 0° C. is added triphenylphosphine (0.451 g, 1.72 mmol), followed by diisopropyl azodicarboxylate (94%, 0.369 g, 1.72 mmol). After 1 hour the mixture is diluted with ethyl acetate and washed with water. The organic phase is dried over MgSO4, filtered and concentrated. The resulting residue is purified by silica gel chromatography (elution with hexanes-ethyl acetate mixtures) to give 3-(7-cyano-1,2,3,4-tetrahydro-naphthalen-1-yl)-3H-imidazole-4-carboxylic acid isopropyl ester; MS: (ESI) m/z 310.1 (M+H)+. The HCl salt of the title compound can be prepared by dissolution in diethyl ether followed by treatment with an excess of 1N HCl in diethyl ether. The resulting heterogeneous solution is concentrated to furnish the HCl salt of 3-(7-cyano-1,2,3,4-tetrahydro-naphthalen-1-yl)-3H-imidazole-4-carboxylic acid isopropyl ester; 1H NMR (400 MHz, MeOD) δ ppm 1.36 (d, J=6.1 Hz, 3 H), 1.39 (d, J=6.3 Hz, 3 H), 1.90-1.98 (m, 2 H), 2.29-2.33 (m, 2 H), 2.97 (dt, J=17.7, 6.3 Hz, 1 H), 3.12 (dd, J=17.7, 6.8 Hz, 1 H), 5.21 (sept, J=6.3 Hz, 1 H), 6.35 (t, J=6.3 Hz, 1 H), 7.25 (s, 1 H), 7.45 (d, J=8.1 Hz, 1 H), 7.59 (s, 1 H), 7.62 (dd, J=8.1, 1.5 Hz, 1 H), 7.78 (d, J=1.5 Hz, 1 H).

Aufarbeitung

  1. customcan be prepared
  2. washwashed with water
  3. dry with materialThe organic phase is dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe resulting residue is purified by silica gel chromatography (elution with hexanes-ethyl acetate mixtures)

Quellen und Nachweise

ORD-Eintrag
ord-56cae0b291b64efa9e224a311740efe4
Quelldatensatz
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08436035B2

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