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1,2-Dichloroethane → N-(3'-hydroxybiphenyl-2-ylmethyl)-2-[3-(4-cyano-3-fluorobenzyl)-3H-imidazol-4-yl]acetamide

HRID 278176
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 278176
[C:1]([C:3]1[CH:18]=[CH:17][C:6]([CH2:7][N:8]2[C:12]([CH2:13][C:14]([O-:16])=O)=[CH:11][N:10]=[CH:9]2)=[CH:5][C:4]=1[F:19])#[N:2].[Li+].Cl.[NH2:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([OH:36])[CH:31]=1.O.ON1C2C=CC=CC=2N=N1.C(Cl)CCl.C(N(C(C)C)CC)(C)C>>[OH:36][C:32]1[CH:31]=[C:30]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=2[CH2:23][NH:22][C:14](=[O:16])[CH2:13][C:12]2[N:8]([CH2:7][C:6]3[CH:17]=[CH:18][C:3]([C:1]#[N:2])=[C:4]([F:19])[CH:5]=3)[CH:9]=[N:10][CH:11]=2)[CH:35]=[CH:34][CH:33]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 5

HCID 111,2-DichloroethaneHCID 81531DiisopropylethylamineHCID 27960291-Hydroxybenzotriazole hydrateHCID 226270902-Aminomethyl-3'-hydroxybiphenyl hydrochlorideHCID 23702864Lithium 1-(4-cyano-3-fluorobenzyl)-imidazol-5-ylacetate

Produkt 1

HCID 22627115
N-(3'-hydroxybiphenyl-2-ylmethyl)-2-[3-(4-cyano-3-fluorobenzyl)-3H-imidazol-4-yl]acetamide

Versuchsvorschrift

A solution of lithium 1-(4-cyano-3-fluorobenzyl)imidazol-5-ylacetate from Step D (143 mg, 0.55 mmol), 2-aminomethyl-3′-hydroxybiphenyl hydrochloride from Example 4, Step H (118 mg, 0.50 mmol), 1-hydroxybenzotriazole hydrate (74 mg, 0.55 mmol), EDC (105 mg, 0.55 mmol), and diisopropylethylamine (129 mg, 1.00 mmol) in dry, degassed DMF (2 mL) was stirred at ambient temperature overnight. The solvent was removed under reduced pressure and the residue was partitioned between sat. aq. NaHCO3 (3 mL) and CHCl3 (5 mL). The aqueous layer was extracted further with CHCl3 (2×5 mL). The combined organic extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by flash column chromatography, eluting with a gradient of 3-5% MeOH/0.3-0.5% NH4OH in CHCl3 to give the titled product as a white foam.

Aufarbeitung

  1. customdegassed DMF (2 mL)
  2. customThe solvent was removed under reduced pressure
  3. customthe residue was partitioned between sat. aq. NaHCO3 (3 mL) and CHCl3 (5 mL)
  4. extractionThe aqueous layer was extracted further with CHCl3 (2×5 mL)
  5. dry with materialThe combined organic extracts were dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by flash column chromatography
  9. washeluting with a gradient of 3-5% MeOH/0.3-0.5% NH4OH in CHCl3

Quellen und Nachweise

ORD-Eintrag
ord-a5bcbe1a98764649acf60c44e5930d77
Quelldatensatz
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06358985B1

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