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Dimethylformamide → N-(2,6-Difluoro-3-hydroxy-phenyl)-5-(3,4-difluorophenyl)-2,3-dimethyl-benzamide

HRID 1771818
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1771818
[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]=[C:11]([CH3:19])[C:12]([CH3:18])=[C:13]([CH:17]=2)[C:14]([OH:16])=O)[CH:5]=[CH:6][C:7]=1[F:8].C(Cl)(C(Cl)=O)=O.CN(C=O)C.[NH2:31][C:32]1[C:33]([F:40])=[C:34]([OH:39])[CH:35]=[CH:36][C:37]=1[F:38].C([O-])(O)=O.[Na+]>C(Cl)Cl.C1COCC1.O>[F:40][C:33]1[C:34]([OH:39])=[CH:35][CH:36]=[C:37]([F:38])[C:32]=1[NH:31][C:14](=[O:16])[C:13]1[CH:17]=[C:9]([C:4]2[CH:5]=[CH:6][C:7]([F:8])=[C:2]([F:1])[CH:3]=2)[CH:10]=[C:11]([CH3:19])[C:12]=1[CH3:18]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 516892Sodium BicarbonateHCID 227559833-Amino-2,4-difluorophenolHCID 894452845-(3,4-Difluorophenyl)-2,3-dimethyl-benzoic acid

Produkt 1

HCID 89443829
N-(2,6-Difluoro-3-hydroxy-phenyl)-5-(3,4-difluorophenyl)-2,3-dimethyl-benzamide
Ausbeute 19 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a solution of 5-(3,4-difluorophenyl)-2,3-dimethyl-benzoic acid (395 mg, 1.51 mmol, 1.1 eq) in CH2Cl2 (5 mL) was added (COCl)2 (521.6 mg, 4.11 mmol, 3.0 eq) dropwise at 0° C. DMF (10 mg, 0.14 mmol, 0.1 eq) was added and the reaction mixture was stirred at room temperature for 2 h. The resulting mixture was concentrated under reduced pressure to remove the solvent and excess reagent. The residue obtained was dissolved in THF (4 mL) and added dropwise to a mixture of 3-amino-2,4-difluoro-phenol (intermediate X(a)) (198 mg, 1.37 mmol, 1.0 eq) and NaHCO3 (575 mg, 6.85 mmol, 5.0 eq) in THF (4 mL) at 0° C. After addition was completed the reaction mixture was stirred at room temperature for 30 min. Water was added and the aqueous layer extracted with EtOAc. The combined organic extracts were washed with saturated NaHCO3, water and brinc, dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified by column chromatography (petroleum ether:EtOAc, 10:1 to 4:1) to give the title compound as a white solid (100 mg, 19%).

Aufarbeitung

  1. concentrationThe resulting mixture was concentrated under reduced pressure
  2. customto remove the solvent and excess reagent
  3. customThe residue obtained
  4. additionAfter addition
  5. stirringwas stirred at room temperature for 30 min
  6. extractionthe aqueous layer extracted with EtOAc
  7. washThe combined organic extracts were washed with saturated NaHCO3, water and brinc
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. customevaporated in vacuo
  11. customThe residue was purified by column chromatography (petroleum ether:EtOAc, 10:1 to 4:1)

Quellen und Nachweise

ORD-Eintrag
ord-62727e5711b943d29c9d8aa54cd9f545
Quelldatensatz
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09249085B2

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