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Aniline → HCID 178511621, Verbindung

HRID 1943479
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1943479
Cl[C:2]1[CH:3]=[C:4]([N:14](CC2C=CC(OC)=CC=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:5]2[N:6]([C:8]([C:11]([OH:13])=O)=[CH:9][N:10]=2)[N:7]=1.[NH2:30][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.C(N(CC)CC)C.[NH2:65][C@H:66]1[CH2:71][CH2:70][C@H:69]([NH2:72])[CH2:68][CH2:67]1>C(Cl)Cl.O.C(#N)C>[NH2:65][C@H:66]1[CH2:71][CH2:70][C@H:69]([NH:72][C:2]2[CH:3]=[C:4]([NH:14][C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:5]3[N:6]([C:8]([C:11]([NH:30][C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)=[O:13])=[CH:9][N:10]=3)[N:7]=2)[CH2:68][CH2:67]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 6115AnilineHCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 596248836-Chloro-8-((4-methoxybenzyl)(phenyl)amino)imidazo[1,2-b]pyridazine-3-carboxylic acidHCID 178511674HCID 178511674, Verbindung

Produkt 1

HCID 178511621HCID 178511621, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittelHCID 21908982Water methylene chlorideLösungsmittel

Versuchsvorschrift

In a 2 dram reaction vial containing acetonitrile (1 mL) at ambient temperature was added 6-chloro-8-((4-methoxybenzyl)(phenyl)amino)imidazo[1,2-b]pyridazine-3-carboxylic acid (0.025 g, 0.06 mmol), aniline (0.008 g, 0.09 mmol), EDCI (0.018 g, 0.09 mmol), HOBt (0.012 g, 0.09 mmol), and triethylamine (0.025 mL, 0.18 mmol). The suspension was stirred overnight at room temperature. The reaction mixture was then concentrated in vacuo and the residue mixed with trans-1,4-diaminocyclohexane (0.5 g, 4.39 mmol) and heated to 160° C. for 5 h. After cooling to room temperature, the reaction mixture was diluted with DCM/water and the layers separated. The organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was dissolved in DCM (1 mL) at room temperature and charged with TFA (1 mL). The mixture stirred 3 h, whereupon the volatiles were removed via a stream of nitrogen and the crude mixture was purified via preparative HPLC (Waters Sunfire column 5u, 100 A, 19×100 mm, 20-100% Solvent B, (Solvent A (90% water, 10% methanol, 0.1% TFA), Solvent B (10% water, 90% methanol, 0.1% TFA), 10 min gradient, 10 minute run, 25 mL/min), affording the title compound, 6-((trans)-4-aminocyclohexylamino)-N-phenyl-8-(phenylamino)imidazo[1,2-b]pyridazine-3-carboxamide. HPLC: Rt=3.02 min. (Waters sunfire 4.6×50 mm C18.5 um 4 min/1 min hold time 0-100% (A-B) A=10% MeOH-90% water-0.1% TFA, B=90% MeOH-10% water-0.1% TFA). MS: [M+H]=442.

Aufarbeitung

  1. customIn a 2 dram reaction
  2. concentrationThe reaction mixture was then concentrated in vacuo
  3. temperatureheated to 160° C. for 5 h
  4. temperatureAfter cooling to room temperature
  5. customthe layers separated
  6. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. dissolutionThe residue was dissolved in DCM (1 mL) at room temperature
  10. additioncharged with TFA (1 mL)
  11. stirringThe mixture stirred 3 h, whereupon the volatiles
  12. customwere removed via a stream of nitrogen
  13. customthe crude mixture was purified via preparative HPLC (Waters Sunfire column 5u, 100 A, 19×100 mm, 20-100% Solvent B, (Solvent A (90% water, 10% methanol, 0.1% TFA), Solvent B (10% water, 90% methanol, 0.1% TFA), 10 min gradient, 10 minute run, 25 mL/min),

Quellen und Nachweise

ORD-Eintrag
ord-dee264ff821549aa87bea70cbe8f49f7
Quelldatensatz
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08389527B2

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