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Sodium hydride → 3-Tert-butyl-isoxazole-5-carboxylic acid [4-chloro-3-nitro-6-(2-trifluoromethyl-phenyl)-pyridin-2-yl]-amide

HRID 1191197
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Reaktionsgleichung

Reaktionsgleichung von HRID 1191197
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[C:14]([F:17])([F:16])[F:15])[N:5]=[C:4]([NH2:18])[C:3]=1[N+:19]([O-:21])=[O:20].[H-].[Na+].[C:24]([C:28]1[CH:32]=[C:31]([C:33](O)=[O:34])[O:30][N:29]=1)([CH3:27])([CH3:26])[CH3:25].C(Cl)(=O)C(Cl)=O>C1COCC1.C(Cl)Cl.CN(C=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[C:14]([F:15])([F:17])[F:16])[N:5]=[C:4]([NH:18][C:33]([C:31]2[O:30][N:29]=[C:28]([C:24]([CH3:27])([CH3:26])[CH3:25])[CH:32]=2)=[O:34])[C:3]=1[N+:19]([O-:21])=[O:20]
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Komponenten

8

Edukt 4

HCID 24758Sodium hydrideHCID 65578Oxalyl chlorideHCID 216484973-Tert-butyl-1,2-oxazole-5-carboxylic acidHCID 674111324-Chloro-3-nitro-6-(2-trifluoromethyl-phenyl)-pyridin-2-ylamine

Produkt 1

HCID 674109013-Tert-butyl-isoxazole-5-carboxylic acid [4-chloro-3-nitro-6-(2-trifluoromethyl-phenyl)-pyridin-2-yl]-amide

Reagenzien, Katalysatoren, Lösungsmittel

3
HCID 6228DimethylformamideKatalysatorHCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 4-chloro-3-nitro-6-(2-trifluoromethyl-phenyl)-pyridin-2-ylamine (100 mg, 0.315 mmol, prepared as described in Example 1, Step B above) in THF (10 mL) was treated with NaH (37.8 mg, 0.944 mmol, 60% dispersion in oil), and the mixture was allowed to stir at room temperature for 1 h. Simultaneously, a solution of 3-tert-butyl-isoxazole-5-carboxylic acid (69.2 mg, 0.409 mmol, prepared as described in Example I above) in DCM (10 mL) was treated with oxalyl chloride (35.7 μL, 0.409 mmol) and DMF (2 drops), and the resulting mixture was stirred at room temperature for 1 h. Volatile components were removed in vacuo, and the residue was taken up in anhydrous THF (6 mL). The above-prepared acid chloride solution was added to the sodium anilide solution above, and the resulting mixture was stirred at room temperature for 15 min. The resulting mixture was then quenched with saturated aqueous NH4Cl (20 mL) and extracted twice with EtOAc (30 mL). The combined organic extracts were dried over MgSO4 and concentrated in vacuo. The residue was purified on a 25-g SEPRA Si 50 SPE column (Flow rate=20 mL/min; Eluent=EtOAc-hexanes, 1:99 for 10 min, then 1:99 to 1:3 over 40 min) to yield 3-tert-butyl-isoxazole-5-carboxylic acid [4-chloro-3-nitro-6-(2-trifluoromethyl-phenyl)-pyridin-2-yl]-amide as a yellow solid. Mass Spectrum (LCMS, ESI pos.): Calculated for C21H16N4O4ClF3: 469.1 (M+H); Measured: 469.1.

Aufarbeitung

  1. stirringthe resulting mixture was stirred at room temperature for 1 h
  2. customVolatile components were removed in vacuo
  3. additionThe above-prepared acid chloride solution was added to the sodium anilide solution above, and the resulting mixture
  4. stirringwas stirred at room temperature for 15 min
  5. customThe resulting mixture was then quenched with saturated aqueous NH4Cl (20 mL)
  6. extractionextracted twice with EtOAc (30 mL)
  7. dry with materialThe combined organic extracts were dried over MgSO4
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified on a 25-g SEPRA Si 50 SPE column (Flow rate=20 mL/min
  10. waitEluent=EtOAc-hexanes, 1:99 for 10 min

Quellen und Nachweise

ORD-Eintrag
ord-592737f1c24a418fa10ef9351589fe87
Quelldatensatz
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08680098B2

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