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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → N-(2-(5-(3,4-dichlorophenyl)furan-2-yl)ethyl)-3-(pyridin-4-yl)-1H-pyrazole-5-carboxamide

HRID 872454
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 872454
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[CH2:8][C:9]([C:12]([OH:14])=O)=[N:10][N:11]=2)=[CH:3][CH:2]=1.CCN(C(C)C)C(C)C.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.Cl.[Cl:46][C:47]1[CH:48]=[C:49]([C:54]2[O:58][C:57]([CH2:59][CH2:60][NH2:61])=[CH:56][CH:55]=2)[CH:50]=[CH:51][C:52]=1[Cl:53]>C(Cl)Cl>[Cl:46][C:47]1[CH:48]=[C:49]([C:54]2[O:58][C:57]([CH2:59][CH2:60][NH:61][C:12]([C:9]3[NH:10][N:11]=[C:7]([C:4]4[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=4)[CH:8]=3)=[O:14])=[CH:56][CH:55]=2)[CH:50]=[CH:51][C:52]=1[Cl:53]
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Komponenten

7

Edukt 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531Diisopropylethylamine2×HCID 27716315-pyridin-4-yl-4H-pyrazole-3-carboxylic acidHCID 671683442-(5-(3,4-Dichlorophenyl)furan-2-yl)ethanamine hydrochloride

Produkt 1

HCID 67174943
N-(2-(5-(3,4-dichlorophenyl)furan-2-yl)ethyl)-3-(pyridin-4-yl)-1H-pyrazole-5-carboxamide
Ausbeute 29,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel3×

Versuchsvorschrift

To a stirred solution of 5-pyridin-4-yl-4H-pyrazole-3-carboxylic acid (1.78 g, 9.42 mmol) in DCM (10 ml) was added DIPEA (2.46 ml, 14.1 mmol), EDCI (2.71 g, 9.42 mmol) and HOBt (1.91, 14.1 mmol). 2-(5-(3,4-dichlorophenyl)furan-2-yl)-ethanamine hydrochloride (2.75 g, 9.42 mmol) was dissolved in DCM (15 ml) and DIPEA (1.64 ml, 9.42 mmol). The resulting solution was added to the reaction mixture, which was stirred at RT overnight. The reaction mixture was diluted with DCM and washed with saturated aqueous NaHCO3 solution and water. The organic phase was dried over Na2SO4, evaporated and purified by chromatography (CombiFlash, silica column, eluent 0-15% MeOH/DCM). Product containing fractions were collected, evaporated and crystallized from DCM and re-crystallized from 2% MeOH/DCM and heptane. Thus, 1.18 g (29%) of the title compound was obtained. 1H-NMR (400 MHz; d6-DMSO): δ 2.97 (t, 2H), 3.59 (q, 2H), 6.35 (d, 1H), 7.03 (d, 1H), 7.33 (s, 1H), 7.62 (d, 2H), 7.75 (m, 2H), 7.84 (t, 1H), 8.57 (br s, 1H), 8.63 (m, 2H), 13.95 (s, 1H).

Aufarbeitung

  1. additionThe resulting solution was added to the reaction mixture, which
  2. washwashed with saturated aqueous NaHCO3 solution and water
  3. dry with materialThe organic phase was dried over Na2SO4
  4. customevaporated
  5. custompurified by chromatography (CombiFlash, silica column, eluent 0-15% MeOH/DCM)
  6. additionProduct containing fractions
  7. customwere collected
  8. customevaporated
  9. customcrystallized from DCM
  10. customre-crystallized from 2% MeOH/DCM and heptane

Quellen und Nachweise

ORD-Eintrag
ord-deb3daeeac524b3c92c26b635cf753ea
Quelldatensatz
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08975254B2

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