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Diisopropylethylamine → HCID 178461980, Verbindung

HRID 75322
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 75322
Cl.C([O:9][C:10]1[CH:15]=[C:14]([C:16]2[CH:17]=[C:18]3[N:27]([CH3:28])[CH:26]=[CH:25][C:19]3=[N:20][C:21]=2[C@@H:22]([NH2:24])[CH3:23])[CH:13]=[CH:12][N:11]=1)C1C=CC=CC=1.Cl.N[C@H](C1N=C2C=CN(C)C2=CC=1C1C=CN=C(O)C=1)C.[NH2:50][C:51]1[N:56]=[C:55]([NH2:57])[C:54]([C:58]#[N:59])=[C:53](Cl)[N:52]=1.C(N(C(C)C)C(C)C)C>C(#N)C>[NH2:50][C:51]1[N:56]=[C:55]([NH2:57])[C:54]([C:58]#[N:59])=[C:53]([NH:24][C@H:22]([C:21]2[N:20]=[C:19]3[CH:25]=[CH:26][N:27]([CH3:28])[C:18]3=[CH:17][C:16]=2[C:14]2[CH:13]=[CH:12][N:11]=[C:10]([OH:9])[CH:15]=2)[CH3:23])[N:52]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 81531DiisopropylethylamineHCID 867080212,4-Diamino-6-chloropyrimidine-5-carbonitrileHCID 86708023(S)-1-(6-(2-(benzyloxy)pyridin-4-yl)-1-methyl-1H-pyrrolo[3,2-b]pyridin-5-yl)ethanamine hydrochlorideHCID 178461863HCID 178461863, Verbindung

Produkt 1

HCID 178461980HCID 178461980, VerbindungAusbeute 46,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of (S)-1-(6-(2-(benzyloxy)pyridin-4-yl)-1-methyl-1H-pyrrolo[3,2-b]pyridin-5-yl)ethanamine hydrochloride (155 mg, 0.393 mmol) and (S)-4-(5-(1-aminoethyl)-1-methyl-1H-pyrrolo[3,2-b]pyridin-6-yl)pyridin-2-ol hydrochloride (120 mg, 0.393 mmol) along with 2,4-diamino-6-chloropyrimidine-5-carbonitrile (100 mg, 0.590 mmol) and N-ethyl-N-isopropylpropan-2-amine (0.205 mL, 1.18 mmol) were combined in acetonitrile (6 mL). The reaction mixture was heated in a microwave reactor at 120° C. for 2 hours and then concentrated. The residue was dissolved in MeOH (10 mL). Pd/C (10%, 700 mg) was added and the reaction mixture was maintained under an atmosphere of hydrogen for 30 minutes. The mixture was filtered through Celite and concentrated. The residue was taken up in DMF and purified by preparative HPLC (basic mode) eluting with 20-35% ACN in water. The fractions containing the desired product were combined and concentrated in vacuo to give the title compound (73 mg, 46%). 1H NMR (500 MHz, DMSO-d6) δ ppm 1.22-1.32 (m, 3 H), 3.80 (br s, 3 H), 5.58 (quin, J=6.71 Hz, 1 H), 6.31 (d, J=6.83 Hz, 1 H), 6.48 (br s, 2 H), 6.52-6.63 (m, 5 H), 6.66 (d, J=7.81 Hz, 1 H), 7.52 (d, J=6.35 Hz, 1 H), 7.72 (d, J=2.93 Hz, 1 H), 7.80 (s, 1 H); ESI-MS m/z [M+H]+ calc'd for C20H19N9O, 402; found 402.

Aufarbeitung

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in MeOH (10 mL)
  3. additionPd/C (10%, 700 mg) was added
  4. temperaturethe reaction mixture was maintained under an atmosphere of hydrogen for 30 minutes
  5. filtrationThe mixture was filtered through Celite
  6. concentrationconcentrated
  7. custompurified by preparative HPLC (basic mode)
  8. washeluting with 20-35% ACN in water
  9. additionThe fractions containing the desired product
  10. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-bd34a423c8034c0eba52f025ad0a625a
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08835420B2

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