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

HRID 1269605
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1269605
C(Cl)(=O)C(Cl)=O.CS(C)=O.[CH:11]1([CH2:14][CH2:15]O)[CH2:13][CH2:12]1.C(N(CC)CC)C.Cl.[F:25][C:26]([F:41])([F:40])[C:27]1[CH:32]=[CH:31][C:30]([C:33]2[CH:38]=[CH:37][CH:36]=[C:35]([NH2:39])[CH:34]=2)=[CH:29][CH:28]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(O)(=O)C>C(Cl)Cl.O>[CH:11]1([CH2:14][CH2:15][NH:39][C:35]2[CH:34]=[C:33]([C:30]3[CH:31]=[CH:32][C:27]([C:26]([F:25])([F:40])[F:41])=[CH:28][CH:29]=3)[CH:38]=[CH:37][CH:36]=2)[CH2:13][CH2:12]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 8

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 1376422-Cyclopropylethan-1-olHCID 27827084'-(Trifluoromethyl)-[1,1'-biphenyl]-3-amine
HCID 5049666
Sodium triacetoxyborohydride

Produkt 1

HCID 18448417N-(2-Cyclopropylethyl)-N-[4'-(trifluoromethyl)-1,1'-biphenyl-3-yl]amineAusbeute 64,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel5×

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

To a solution of oxalyl chloride (0.17 mL, 1.95 mmol) in anhydrous CH2Cl2 (5 mL) under nitrogen at −78° C. was added dropwise a solution of anhydrous DMSO (0.18 mL, 2.6 mmol) in anhydrous CH2Cl2 (2.5 mL), ensuring the temperature remained below −60° C. To this was added a solution of 2-cyclopropyl ethanol (0.132 g, 1.3 mmol) in anhydrous CH2Cl2 (2.5 mL), again ensuring temperature remained below −60° C. The reaction mixture was stirred at −78° C. for 20 mins, then treated with triethylamine (0.543 mL, 3.9 mmol) in anhydrous CH2Cl2 (3 mL). The resultant mixture was allowed to gradually warm to room temperature and stirred for 16 h. The reaction mixture was diluted with CH2Cl2 (10 mL) and water (5 mL) prior to the addition of 2M HCl (0.5 mL). The mixture was stirred vigorously for 20 mins, then passed through a hydrophobic frit. The organic solution was stood over molecular sieves for 2 h, then decanted into a clean flask. To this solution was added 4′-(trifluoromethyl)-1,1′-biphenyl-3-ylamine (0.31 g, 1.3 mmol), followed by sodium triacetoxyborohydride (0.386 g, 1.82 mmol) and acetic acid (74.3 μL, 1.3 mmol). The resultant mixture was stirred at room temperature under nitrogen for 20 h. The reaction mixture was quenched with sat. NaHCO3 aq. (15 mL) and extracted with CH2Cl2 (2×20 mL). The organic solution was passed through a hydrophobic frit and the solvent was removed in vacuo. Purification by SPE (20 g Silica column) eluted with 1:200 EtOAc:cyclohexane afforded the title compound as a colourless oil (255 mg).

Aufarbeitung

  1. customremained below −60° C
  2. customremained below −60° C
  3. temperatureto gradually warm to room temperature
  4. stirringstirred for 16 h
  5. stirringThe mixture was stirred vigorously for 20 mins
  6. waitThe organic solution was stood over molecular sieves for 2 h
  7. customdecanted into a clean flask
  8. customThe reaction mixture was quenched with sat. NaHCO3 aq. (15 mL)
  9. extractionextracted with CH2Cl2 (2×20 mL)
  10. customthe solvent was removed in vacuo
  11. customPurification by SPE (20 g Silica column)
  12. washeluted with 1:200 EtOAc

Quellen und Nachweise

ORD-Eintrag
ord-2739f8d78f164d029d8a9c857e62deb7
Quelldatensatz
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07199239B2

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