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1-Hydroxybenzotriazole → 5-(4-Hydroxy-phenyl)-isoxazole-3-carboxylic acid {2-oxo-2-[4-(3-trifluoromethyl-phenoxy)-piperidin-1-yl]-ethyl}-amide

HRID 1093760
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Reaktionsgleichung

Reaktionsgleichung von HRID 1093760
CCN(C(C)C)C(C)C.[OH:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[O:21][N:20]=[C:19]([C:22]([OH:24])=O)[CH:18]=2)=[CH:13][CH:12]=1.C(OC1C=C(C(=O)C)C=CC=1)C1C=CC=CC=1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.Cl.[NH2:65][CH2:66][C:67]([N:69]1[CH2:74][CH2:73][CH:72]([O:75][C:76]2[CH:81]=[CH:80][CH:79]=[C:78]([C:82]([F:85])([F:84])[F:83])[CH:77]=2)[CH2:71][CH2:70]1)=[O:68]>CN(C=O)C.O>[O:68]=[C:67]([N:69]1[CH2:70][CH2:71][CH:72]([O:75][C:76]2[CH:81]=[CH:80][CH:79]=[C:78]([C:82]([F:85])([F:83])[F:84])[CH:77]=2)[CH2:73][CH2:74]1)[CH2:66][NH:65][C:22]([C:19]1[CH:18]=[C:17]([C:14]2[CH:13]=[CH:12][C:11]([OH:10])=[CH:16][CH:15]=2)[O:21][N:20]=1)=[O:24]
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Komponenten

9

Edukt 6

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 986891-(3-(Phenylmethoxy)phenyl)ethan-1-oneHCID 10909835-(4-Hydroxyphenyl)isoxazole-3-carboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 66591547
2-Amino-1-[4-(3-trifluoromethyl-phenoxy)-piperidin-1-yl]-ethanone hydrochloride

Produkt 1

HCID 1361706625-(4-Hydroxy-phenyl)-isoxazole-3-carboxylic acid {2-oxo-2-[4-(3-trifluoromethyl-phenoxy)-piperidin-1-yl]-ethyl}-amideAusbeute 51,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

DIPEA (133 mg, 1.03 mmol) was added to a stirred solution of 5-(4-hydroxy-phenyl)-isoxazole-3-carboxylic acid (61 mg, 0.294 mmol) (prepared by the method used for the synthesis of Intermediate 25, starting from 3′benzyloxyacetophenone) in DMF (2 mL) followed by HOBt (41.7 mg, 0.308 mmol) and EDCI.HCl (59 mg, 0.308 mmol). After 2 minutes 2-amino-1-[4-(3-trifluoromethyl-phenoxy)-piperidin-1-yl]-ethanone hydrochloride (99 mg, 0.294 mmol) (prepared according to Step 1 and 5 of the General Scheme) was added to the reaction mixture and stirring was continued at ambient temperature overnight. The reaction mixture was diluted with cold water, extracted with ethyl acetate, dried over sodium sulfate and concentrated under reduced pressure. Purification by recrystallisation from 110% EtOAc in hexane afforded 74 mg (51.3% Yield) of 5-(4-hydroxy-phenyl)-isoxazole-3-carboxylic acid {2-oxo-2-[4-(3-trifluoromethyl-phenoxy)-piperidin-1-yl]-ethyl}-amide. LC/MS [M+H]+: 490, 90.53%. 1H NMR (300 MHz, DMSO-d6): δ10.2 (s, 1H), 8.6 (s, 1H), 7.78 (d, 2H), 7.5 (t, 1H), 7.3 (t, 3H), 7.16 (s, 1H), 6.9 (m, 2H), 4.7 (m, 1H), 4.2 (d, 2H), 3.9 (m, 1H), 3.7 (m, 1H), 3.4 (m, 2H), 2.0 (m, 2H), 1.6 (m, 2H).

Aufarbeitung

  1. customprepared by the method
  2. additionwas added to the reaction mixture
  3. extractionextracted with ethyl acetate
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customPurification
  7. customby recrystallisation from 110% EtOAc in hexane

Quellen und Nachweise

ORD-Eintrag
ord-5d8e2ad444094b5a9a7c65f130355639
Quelldatensatz
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08129376B2

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