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1,2-Dichloroethane → (R)-2-[1-(4-cyano-3-fluorobenzyl)-1H-imidazol-5-yl]-N-(1-(7-hydroxynaphthalen-1-yl)-2-oxopyrrolidin-3-yl)acetamide

HRID 2306194
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2306194
[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][C@@H:23]1[CH2:27][CH2:26][N:25]([C:28]2[C:37]3[C:32](=[CH:33][CH:34]=[C:35]([OH:38])[CH:36]=3)[CH:31]=[CH:30][CH:29]=2)[C:24]1=[O:39].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.C(N(CC)C(C)C)(C)C>CN(C=O)C>[C:1]([C:3]1[CH:18]=[CH:17][C:6]([CH2:7][N:8]2[C:12]([CH2:13][C:14]([NH:22][C@@H:23]3[CH2:27][CH2:26][N:25]([C:28]4[C:37]5[C:32](=[CH:33][CH:34]=[C:35]([OH:38])[CH:36]=5)[CH:31]=[CH:30][CH:29]=4)[C:24]3=[O:39])=[O:16])=[CH:11][N:10]=[CH:9]2)=[CH:5][C:4]=1[F:19])#[N:2]
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Komponenten

7

Edukt 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 23702864Lithium 1-(4-cyano-3-fluorobenzyl)-imidazol-5-ylacetateHCID 70170731(r)-3-Amino-1-(7-hydroxynaphthalen-1-yl)-2-oxopyrrolidine hydrochloride

Produkt 1

HCID 70171499
(R)-2-[1-(4-cyano-3-fluorobenzyl)-1H-imidazol-5-yl]-N-(1-(7-hydroxynaphthalen-1-yl)-2-oxopyrrolidin-3-yl)acetamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of lithium [1-(4-cyano-3-fluorobenzyl)-1H-imidazol-5-yl]acetate, as described above in Step D, (46 mg, 0.18 mmol), (R)-3-amino-1-(7-hydroxynaphthalen-1-yl)-2-oxopyrrolidine hydrochloride, as described in Example 10A (45 mg, 0.16 mmol), HOBT (24 mg, 0.18 mmol), EDC (35 mg, 0.18 mmol), and N,N-diisopropylethylamine (0.084 mL, 0.48 mmol) was stirred in DMF (1 mL) at ambient temperature for 18 hours. The solvent was removed under reduced pressure and the residue was partitioned between saturated aqueous NaHCO3 (1 mL) and CHCl3 (2 mL). The aqueous layer was extracted further with CHCl3 (2×2 mL). The combined organic extracts were dried over MgSO4, filtered, and concentrated in vacuo. The crude product was purified by flash column chromatography on silica, eluting with a gradient of EtOAc—10% MeOH—1% NH4OH to EtOAc—15% MeOH—1.5% NH4OH to yield the titled product as a white solid.

Aufarbeitung

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was partitioned between saturated aqueous NaHCO3 (1 mL) and CHCl3 (2 mL)
  3. extractionThe aqueous layer was extracted further with CHCl3 (2×2 mL)
  4. dry with materialThe combined organic extracts were dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe crude product was purified by flash column chromatography on silica
  8. washeluting with a gradient of EtOAc—10% MeOH—1% NH4OH to EtOAc—15% MeOH—1.5% NH4OH

Quellen und Nachweise

ORD-Eintrag
ord-73c49428795640b78f201b8877d5f99a
Quelldatensatz
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06441017B1

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