Trifluoroacetic acid → HCID 178522004, Verbindung

HRID 1521770Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1521770
[O:1]=[C:2]1[NH:8][CH2:7][CH2:6][CH2:5][N:4]2[C:9]3[N:15]=[C:14]([C:16]([NH:18][C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([C:25]5[N:26]=[CH:27][N:28](C(C6C=CC=CC=6)(C6C=CC=CC=6)C6C=CC=CC=6)[CH:29]=5)[CH:20]=4)=[O:17])[CH:13]=[CH:12][C:10]=3[CH:11]=[C:3]12.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH:28]1[CH:29]=[C:25]([C:21]2[CH:20]=[C:19]([NH:18][C:16]([C:14]3[CH:13]=[CH:12][C:10]4[CH:11]=[C:3]5[C:2](=[O:1])[NH:8][CH2:7][CH2:6][CH2:5][N:4]5[C:9]=4[N:15]=3)=[O:17])[CH:24]=[CH:23][CH:22]=2)[N:26]=[CH:27]1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 672372246-oxo-N-[3-(1-trityl-1H-imidazol-4-yl)phenyl]-7,8,9,10-tetrahydro-6H-pyrido[3',2':4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxamide

Produkt 1

HCID 178522004HCID 178522004, VerbindungAusbeute 47 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 6-oxo-N-[3-(1-trityl-1H-imidazol-4-yl)phenyl]-7,8,9,10-tetrahydro-6H-pyrido[3′,2′:4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxamide (86 mg, 0.14 mmol) in CH2Cl2 (1 mL) is added TFA (0.5 mL). The mixture is stirred at room temperature for 16 hr then is concentrated under reduced pressure. The residue is purified via preparative HPLC using a gradient elution from 10-75% acetonitrile/H2O with 0.1% TFA to afford the title compound (25 mg, 47%). LCMS: 387.86 (M+H+). (System T-med polar) Table 3 below, lists the mass spectral data and the HPLC retention times for Examples 1 to 105.

Aufarbeitung

  1. concentrationthen is concentrated under reduced pressure
  2. customThe residue is purified via preparative HPLC
  3. washa gradient elution from 10-75% acetonitrile/H2O with 0.1% TFA

Quellen und Nachweise

ORD-Eintrag
ord-38eec52f48b748628f162095f25007be
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09073926B2

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