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Ethylenediamine → HCID 71288385, Verbindung

HRID 246150
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 246150
[CH3:1][O:2][CH2:3][C@H: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]([Cl: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].C(O)(C(F)(F)F)=O.C(N)CN>ClCCl>[CH3:1][O:2][CH2:3][C@H: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]([Cl: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]
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Komponenten

5

Edukt 3

HCID 3301EthylenediamineHCID 6422Trifluoroacetic acidHCID 712860582-(6-chloro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid ((R)-2-methoxy-1-methyl-ethyl)-amide

Produkt 1

HCID 71288385HCID 71288385, VerbindungAusbeute 59 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344
Dichloromethane
Lösungsmittel

Versuchsvorschrift

In a sealed 25 mL round-bottom flask, 2-(6-chloro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid ((R)-2-methoxy-1-methyl-ethyl)-amide (32 mg, 0.061 mmol) and TFA (0.9 ml, 11.7 mmol) were combined with dichloromethane (3 ml) to give an orange solution. The reaction mixture was stirred at room temperature until the consumption of starting material (2.5 h). The reaction mixture was then concentrated under reduced pressure. The resultant crude solid was dissolved in dichloromethane (3 mL) and ethylenediamine (300 μl, 4.44 mmol) was added. The reaction mixture was stirred at room temperature for 18 h. The reaction mixture was concentrated and the residue was precipitated with water. The suspension was stirred for 1 h and the crude solid collected by filtration. The crude solid was purified by trituration (1:1 dichloromethane/heptane) to afford 14 mg (59%) of 2-(6-chloro-1-methyl-1H-indazol-3-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid ((R)-2-methoxy-1-methyl-ethyl)-amide as an off-white solid. MS: [M+H]+=399; 1H NMR (300 MHz, DMSO-d6) δ: 9.11 (s, 1H), 8.53 (d, J=8.6 Hz, 1H), 8.44 (s, 1H), 8.20 (d, J=8.6 Hz, 1H), 8.01 (d, J=1.5 Hz, 1H), 7.28 (dd, J=8.6, 2.0 Hz, 1H), 4.30-4.46 (m, 1H), 4.18 (s, 3H), 3.53 (dd, J=9.6, 5.1 Hz, 1H), 3.47 (dd, J=9.6, 4.5 Hz, 1H), 3.27 (s, 3H), 1.31 (d, J=6.6 Hz, 3H).

Aufarbeitung

  1. customto give an orange solution
  2. concentrationThe reaction mixture was then concentrated under reduced pressure
  3. dissolutionThe resultant crude solid was dissolved in dichloromethane (3 mL)
  4. stirringThe reaction mixture was stirred at room temperature for 18 h
  5. concentrationThe reaction mixture was concentrated
  6. customthe residue was precipitated with water
  7. stirringThe suspension was stirred for 1 h
  8. filtrationthe crude solid collected by filtration
  9. customThe crude solid was purified by trituration (1:1 dichloromethane/heptane)

Quellen und Nachweise

ORD-Eintrag
ord-fd48dc3f605742f5990f90a21aa26ae9
Quelldatensatz
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08658646B2

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