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Acetic Acid → N-Butyl-N-[2-methyl-4'-(trifluoromethyl)-1,1'-biphenyl-3-yl]amine

HRID 1269614
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1269614
CO[CH:3](OC)[CH2:4]OC.Cl.[CH3:10][C:11]1[C:16]([NH2:17])=[CH:15][CH:14]=[CH:13][C:12]=1[C:18]1[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][CH:19]=1.[C:28](O[BH-](OC(=O)C)OC(=O)C)(=O)[CH3:29].[Na+].C(O)(=O)C.C(=O)(O)[O-].[Na+]>>[CH2:28]([NH:17][C:16]1[C:11]([CH3:10])=[C:12]([C:18]2[CH:23]=[CH:22][C:21]([C:24]([F:25])([F:26])[F:27])=[CH:20][CH:19]=2)[CH:13]=[CH:14][CH:15]=1)[CH2:29][CH2:4][CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 6

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 475201,1,2-TrimethoxyethaneHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 184483532-Methyl-4'-(trifluoromethyl)biphenyl-3-amine

Produkt 1

HCID 18448423
N-Butyl-N-[2-methyl-4'-(trifluoromethyl)-1,1'-biphenyl-3-yl]amine

Versuchsvorschrift

1,1,2-trimethoxyethane (0.162 mL, 1.26 mL) was added to 0.5N HCl (2.52 mL, 1.26 mmol) and the resultant solution heated for 1 h at 50° C. The cooled reaction mixture was extracted with CH2Cl2. The organic solution was passed through a hydrophobic frit, dried for 2 h (3A molecular sieves). 2-Methyl-4′-(trifluoromethyl)-1,1′-biphenyl-3-ylamine (0.32 g, 1.26 mmol) was added to the organic solution and the solution stirred for 20 min at rt. Sodium triacetoxyborohydride (0.325 g, 1.77 mmol) and acetic acid (0.072 mL, 1.26 mmol) were then added, and the resultant mixture stirred for 16 h at rt. Saturated sodium bicarbonate was added to the reaction mixture and once effervescence had ceased the mixture was extracted with CH2Cl2. The organic solution was passed through a hydrophobic frit and the solvents removed in vacuo. Purification by Biotage™ chromatography (silica, 40 g) eluted with 10% EtOAc/cyclohexane afforded the title compound (42 mg).

Aufarbeitung

  1. customThe cooled reaction mixture
  2. extractionwas extracted with CH2Cl2
  3. dry with materialdried for 2 h (3A molecular sieves)
  4. extractionwas extracted with CH2Cl2
  5. customthe solvents removed in vacuo
  6. customPurification by Biotage™ chromatography (silica, 40 g)
  7. washeluted with 10% EtOAc/cyclohexane

Quellen und Nachweise

ORD-Eintrag
ord-e76dd292ae334ae4a850d01cff624311
Quelldatensatz
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07199239B2

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