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Trifluoroacetic acid → HCID 69933247, Verbindung

HRID 540797
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 540797
[F:1][C:2]([F:40])([F:39])[C:3]1[CH:38]=[CH:37][C:6]([O:7][C:8]2[N:12]([CH2:13][C:14]([N:16]([CH3:18])[CH3:17])=[O:15])[N:11]=[C:10]([C:19]3[CH:20]=[C:21]([C:25]4([NH:29]C(=O)OC(C)(C)C)[CH2:28][O:27][CH2:26]4)[CH:22]=[CH:23][CH:24]=3)[CH:9]=2)=[CH:5][CH:4]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:29][C:25]1([C:21]2[CH:20]=[C:19]([C:10]3[CH:9]=[C:8]([O:7][C:6]4[CH:5]=[CH:4][C:3]([C:2]([F:1])([F:39])[F:40])=[CH:38][CH:37]=4)[N:12]([CH2:13][C:14]([N:16]([CH3:18])[CH3:17])=[O:15])[N:11]=3)[CH:24]=[CH:23][CH:22]=2)[CH2:28][O:27][CH2:26]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 69932959HCID 69932959, Verbindung

Produkt 1

HCID 69933247HCID 69933247, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A stirred solution of tert-butyl [3-(3-{5-(4-trifluoromethylphenoxy)-1-[2-(dimethylamino)-2-oxoethyl]-1H-pyrazol-3-yl}phenyl)oxetan-3-yl]carbamate (70 mg, 0.13 mmol) in 2 mL of CH2Cl2 was cooled in an ice bath. To the solution was added 1 mL of TFA and the mixture was stirred for 1 h. The cooling bath was removed and the mixture was stirred at ambient temperature for 1 h. 10% Aqueous Na2CO3 solution was added and the mixture was extracted with CH2Cl2. The combined organic phases were dried over Na2SO4, filtered, and the solvent was removed under reduced pressure to give 2-{3-[3-(3-aminooxetan-3-yl)phenyl]-5-(4-trifluoromethylphenoxy)-1H-pyrazol-1-yl}-N,N-dimethylacetamide as an oil. Calcd (M+1)+: 461.4. Found: 461.5

Aufarbeitung

  1. customThe cooling bath was removed
  2. stirringthe mixture was stirred at ambient temperature for 1 h
  3. addition10% Aqueous Na2CO3 solution was added
  4. extractionthe mixture was extracted with CH2Cl2
  5. dry with materialThe combined organic phases were dried over Na2SO4
  6. filtrationfiltered
  7. customthe solvent was removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6c29bf2ee8734986b24e5f3af6db96b8
Quelldatensatz
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08871796B2

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