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Acetonitrile → HCID 71285744, Verbindung

HRID 246186
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 246186
[OH:1][C:2]([CH3:38])([CH3:37])[CH2:3][CH:4]([NH:6][C:7]([C:9]1[C:17]2[C:12](=[N:13][CH:14]=[C:15]([C:18]3[C:26]4[C:21](=[CH:22][C:23]([F:27])=[CH:24][CH:25]=4)[N:20]([CH3:28])[N:19]=3)[N:16]=2)[N:11](COCC[Si](C)(C)C)[CH:10]=1)=[O:8])[CH3:5].[F-].[Cs+].C1OCCOCCOCCOCCOCCOC1.C(#N)C>C(OCC)(=O)C>[OH:1][C:2]([CH3:37])([CH3:38])[CH2:3][CH:4]([NH:6][C:7]([C:9]1[C:17]2[C:12](=[N:13][CH:14]=[C:15]([C:18]3[C:26]4[C:21](=[CH:22][C:23]([F:27])=[CH:24][CH:25]=4)[N:20]([CH3:28])[N:19]=3)[N:16]=2)[NH:11][CH:10]=1)=[O:8])[CH3:5]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 6342AcetonitrileHCID 25953Cesium fluoride2×HCID 2855718-Crown-62×HCID 712857852-(6-fluoro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid (3-hydroxy-1,3-dimethyl-butyl)-amide

Produkt 1

HCID 71285744HCID 71285744, Verbindung
Ausbeute 21,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

In a 125 mL round-bottomed flask, 2-(6-fluoro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid (3-hydroxy-1,3-dimethyl-butyl)-amide (25 mg, 0.046 mmol), cesium fluoride (70 mg, 0.46 mmol) and 18-crown-6 (12 mg, 0.046 mmol) were combined with acetonitrile to give an off-white suspension. The reaction was stirred at reflux for 72 h. A large excess of CsF and 18-crown-6 was added and the reaction was heated for an additional 24 h. The reaction mixture was diluted with ethyl acetate and washed with water. The organic layer was dried over Na2SO4 and concentrated. The crude material was suspended in water and collected by filtration then triturated with 1:2 dichloromethane/heptane to afford 4 mg (21%) of 2-(6-fluoro-1-methyl-1H-indazol-3-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid (3-hydroxy-1,3-dimethyl-butyl)-amide as a yellow solid. MS: [M+Na]+=433, 1H NMR (300 MHz, DMSO-d6) δ: 12.83 (br. s., 1H), 9.10 (s, 1H), 8.57 (dd, J=8.9, 5.5 Hz, 1H), 8.41 (d, J=2.3 Hz, 1H), 8.15 (d, J=8.3 Hz, 1H), 7.71 (dd, J=9.8, 1.9 Hz, 1H), 7.20 (td, J=9.1, 2.3 Hz, 1H), 4.35 (s, 1H), 4.29-4.43 (m, 1H), 4.16 (s, 3H), 1.83 (dd, J=14.4, 7.9 Hz, 1H), 1.73 (dd, J=16.6, 4.9 Hz, 1H), 1.31 (d, J=6.4 Hz, 3H), 1.15 (s, 3H), 1.12 (s, 3H).

Aufarbeitung

  1. customto give an off-white suspension
  2. temperatureat reflux for 72 h
  3. temperaturethe reaction was heated for an additional 24 h
  4. washwashed with water
  5. dry with materialThe organic layer was dried over Na2SO4
  6. concentrationconcentrated
  7. filtrationcollected by filtration
  8. customthen triturated with 1:2 dichloromethane/heptane

Quellen und Nachweise

ORD-Eintrag
ord-879ff8395eb448bd964269db4e02fbeb
Quelldatensatz
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08658646B2

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