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Oxalyl chloride → HCID 86682247, Verbindung

HRID 1428376
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1428376
[CH3:1][S:2][CH:3]([CH3:7])[C:4](O)=[O:5].C(Cl)(=O)C(Cl)=O.[Cl:14][C:15]1[C:19]([NH:20][CH2:21][C:22]#[CH:23])=[CH:18][N:17]([C:24]2[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=2)[N:16]=1.C(N(C(C)C)C(C)C)C>C(Cl)Cl.CN(C=O)C>[Cl:14][C:15]1[C:19]([N:20]([CH2:21][C:22]#[CH:23])[C:4](=[O:5])[CH:3]([S:2][CH3:1])[CH3:7])=[CH:18][N:17]([C:24]2[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=2)[N:16]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 100851S-Methylthiolactic acidHCID 86682245HCID 86682245, Verbindung

Produkt 1

HCID 86682247HCID 86682247, VerbindungAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228
Dimethylformamide
Katalysator
HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of 2-(methylthio)propanoic acid (0.36 g, 3.00 mmol) in DCM (3 mL) was added oxalyl dichloride (0.29 ml, 3.31 mmol) followed by one drop of DMF. The reaction mixture was stirred for 30 min before all of the solvent was evaporated. The resulting residue was dissolved in DCM (2 mL) and the solution was added to a pre-stirred solution of 3-chloro-N-(prop-2-yn-1-yl)-1-(pyridin-3-yl)-1H-pyrazol-4-amine (0.35 g, 1.50 mmol) and N-ethyl-N-isopropylpropan-2-amine (0.57 ml, 3.31 mmol) in DCM (5.5 mL). The reaction mixture was stirred at ambient temperature for 16 h. The reaction mixture was concentrated and the residue was purified using silica gel chromatography (0-100% EtOAc/hexanes) to afford the title compound as a yellow oil (432 mg, 1.23 mmol, 85%): 1H NMR (400 MHz, CDCl3) δ 8.97 (d, J=2.5 Hz, 1H), 8.66-8.60 (m, 1H), 8.25 (s, 1H), 8.08-8.01 (m, 1H), 7.49-7.42 (m, 1H), 4.86 (s, 1H), 4.29-3.97 (m, 1H), 3.31 (d, J=6.5 Hz, 1H), 2.30-2.24 (m, 1H), 2.09 (s, 3H), 1.46 (d, J=6.9 Hz, 3H); 13C NMR (101 MHz, CDCl3) δ 171.30, 148.66, 140.71, 140.18, 135.71, 127.87, 126.35, 124.11, 122.12, 78.53, 72.92, 53.39, 37.97, 16.42, 11.07; ESIMS m/z 335 ([M+H]+).

Aufarbeitung

  1. customwas evaporated
  2. dissolutionThe resulting residue was dissolved in DCM (2 mL)
  3. stirringThe reaction mixture was stirred at ambient temperature for 16 h
  4. concentrationThe reaction mixture was concentrated
  5. customthe residue was purified

Quellen und Nachweise

ORD-Eintrag
ord-e5196051d2e14f3b9ed9668935c1d5ce
Quelldatensatz
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08937083B2

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