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Trifluoroacetic acid → 1-[4-[6-Amino-5-(1,3-benzoxazol-2-yl)-3-pyridyl]-1-(4-piperidyl)pyrazol-3-yl]ethanol

HRID 908466
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 908466
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[C:9]([CH:26]([OH:28])[CH3:27])=[N:10][N:11]([CH:13]3[CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH2:14]3)[CH:12]=2)=[CH:4][C:3]=1[C:29]1[O:30][C:31]2[CH:37]=[CH:36][CH:35]=[CH:34][C:32]=2[N:33]=1.FC(F)(F)C(O)=O>ClCCl>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[C:9]([CH:26]([OH:28])[CH3:27])=[N:10][N:11]([CH:13]3[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[CH:12]=2)=[CH:4][C:3]=1[C:29]1[O:30][C:31]2[CH:37]=[CH:36][CH:35]=[CH:34][C:32]=2[N:33]=1
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Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 67388061Tert-butyl 4-[4-[6-amino-5-(1,3-benzoxazol-2-yl)-3-pyridyl]-3-(1-hydroxyethyl)pyrazol-1-yl]piperidine-1-carboxylate

Produkt 1

HCID 576871241-[4-[6-Amino-5-(1,3-benzoxazol-2-yl)-3-pyridyl]-1-(4-piperidyl)pyrazol-3-yl]ethanolAusbeute 80,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Tert-butyl 4-[4-[6-amino-5-(1,3-benzoxazol-2-yl)-3-pyridyl]-3-(1-hydroxyethyl)pyrazol-1-yl]piperidine-1-carboxylate (0.17 g) dissolved in dichloromethane (1 ml) was treated with trifluoroacetic acid (2 ml) and stirred at room temperature for 2 hours. The resulting mixture was evaporated to dryness and the residual trifluoroacetic acid was removed by azeotropic distillation with toluene under vacuum to afford the crude product. The crude product was purified by flash chromatography on silica gel eluting with 0 to 10% methanolic ammonia (7 N) in dichloromethane. The solvent was evaporated to dryness and the yellow foam was triturated with acetonitrile and re-evaporated to dryness to afford 1-[4-[6-amino-5-(1,3-benzoxazol-2-yl)-3-pyridyl]-1-(4-piperidyl)pyrazol-3-yl]ethanol (0.110 g) as a solid. NMR Spectrum: (DMSOd6): 1.43 (d, 1.5H), 1.44 (d, 1.5H), 1.74-1.86 (m, 1H), 1.93-2.03 (m, 2H), 2.03-2.09 (m, 1H), 2.09-2.17 (m, 1H), 2.56-2.64 (m, 1H), 3.01-3.08 (m, 1H), 3.10-3.18 (m, 1H), 4.10-4.20 (m, 1H), 4.78-4.87 (m, 1H), 5.21 (d, 0.5H), 5.22 (d, 0.5H), 7.40-7.48 (m, 2H), 7.63 (bs, 2H), 7.77 (dd, 1H), 7.84 (dd, 1H), 8.04 (s, 0.5H), 8.11 (s, 0.5H), 7.51 (d, 0.5H), 7.52 (d, 0.5H), 7.56 (d, 0.5H), 7.57 (d, 0.5H); Mass spectrum: M+H+ 405.

Aufarbeitung

  1. customThe resulting mixture was evaporated to dryness
  2. customthe residual trifluoroacetic acid was removed by azeotropic distillation with toluene under vacuum
  3. customto afford the crude product
  4. customThe crude product was purified by flash chromatography on silica gel eluting with 0 to 10% methanolic ammonia (7 N) in dichloromethane
  5. customThe solvent was evaporated to dryness
  6. customthe yellow foam was triturated with acetonitrile
  7. customre-evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-f9c038c83dcf42858d5106e846b15f43
Quelldatensatz
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08017611B2

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