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Ozone → 4-[2-(4-tert-Butyl-phenyl)-3H-imidazo[4,5-c]pyridin-7-yl]-piperazine-1-carboxylic acid benzyl ester

HRID 729355
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 729355
[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH:14]=[CH:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O=[O+][O-].P(OCC)(OCC)OCC.[C:29]([C:33]1[CH:38]=[CH:37][C:36]([C:39]2[NH:40][C:41]3[C:46]([NH2:47])=[CH:45][N:44]=[CH:43][C:42]=3[N:48]=2)=[CH:35][CH:34]=1)([CH3:32])([CH3:31])[CH3:30].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C(Cl)Cl.CO>[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH2:14][N:47]([C:46]2[C:41]3[N:40]=[C:39]([C:36]4[CH:37]=[CH:38][C:33]([C:29]([CH3:32])([CH3:31])[CH3:30])=[CH:34][CH:35]=4)[NH:48][C:42]=3[CH:43]=[N:44][CH:45]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 24823OzoneHCID 31215Triethyl phosphiteHCID 643471Benzyl 3-pyrroline-1-carboxylateHCID 5049666Sodium triacetoxyborohydrideHCID 178440764HCID 178440764, Verbindung

Produkt 1

HCID 57832760
4-[2-(4-tert-Butyl-phenyl)-3H-imidazo[4,5-c]pyridin-7-yl]-piperazine-1-carboxylic acid benzyl ester
Ausbeute 2,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

2,5-Dihydro-pyrrole-1-carboxylic acid benzyl ester 6 was dissolved in DCM (5 ml) and MeOH (2 ml). It was cooled to −78° C. and treated with ozone until it was blue in color. Triethyl phosphite (246 mg, 1.48 mmol) was added and the solution was allowed to stir for 5 minutes. 2-(4-tert-Butyl-phenyl)-1H-imidazo[4,5-c] pyridin-7-ylamine 4 (266 mg, 1.00 mmol) was added followed by sodium triacetoxyborohydride (538 mg, 2.54 mmol). This mixture was allowed to stir for 18 hours. Mass spectroscopy showed no starting material left after this time, and the solvent was removed under vacuum. The crude was taken up in ethyl acetate and washed with a saturated sodium bicarbonate solution, brine, dried over MgSO4, and the crude was purified by HPLC (Method E), yielding the title product 7 (12 mg (2.5%), 0.026 mmol). 1H NMR (DMSO-d6): δ 8.88 (bs, 1H), 8.23 (d, J=8.5 Hz, 2H), 7.96 (s, 1H), 7.68 (d, J=8.5 Hz, 2H), 7.38 (m, 5H), 5.15 (s, 2H), 1.33 (s, 9H). MS (ESI-POS): [M+H]+=470; MS(ESI-NEG):[M−H]−=468.

Aufarbeitung

  1. stirringto stir for 18 hours
  2. waitleft after this time
  3. customthe solvent was removed under vacuum
  4. washwashed with a saturated sodium bicarbonate solution, brine
  5. dry with materialdried over MgSO4
  6. customthe crude was purified by HPLC (Method E)

Quellen und Nachweise

ORD-Eintrag
ord-ad390ac47f0c4b5e9dc6f68d48e90946
Quelldatensatz
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07582634B2

Notizen zur Reaktion

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