Trifluoroacetic acid → HCID 68515987, Verbindung

HRID 2241353Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2241353
[CH3:1][O:2][C:3]1[CH:57]=[CH:56][C:6]([CH2:7][N:8]2[C:12]3=[N:13][CH:14]=[CH:15][C:16]([O:17][C:18]4[CH:23]=[CH:22][C:21]([NH:24][C:25]([C:27]5[C:32](=[O:33])[N:31]([C:34]6[CH:39]=[CH:38][C:37]([F:40])=[CH:36][CH:35]=6)[N:30]=[CH:29][CH:28]=5)=[O:26])=[CH:20][C:19]=4[F:41])=[C:11]3[C:10]([N:42]3[CH2:48][CH2:47][CH2:46][N:45](C(OC(C)(C)C)=O)[CH2:44][CH2:43]3)=[N:9]2)=[CH:5][CH:4]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[N:42]1([C:10]2[C:11]3[C:12](=[N:13][CH:14]=[CH:15][C:16]=3[O:17][C:18]3[CH:23]=[CH:22][C:21]([NH:24][C:25]([C:27]4[C:32](=[O:33])[N:31]([C:34]5[CH:39]=[CH:38][C:37]([F:40])=[CH:36][CH:35]=5)[N:30]=[CH:29][CH:28]=4)=[O:26])=[CH:20][C:19]=3[F:41])[N:8]([CH2:7][C:6]3[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:57][CH:56]=3)[N:9]=2)[CH2:48][CH2:47][CH2:46][NH:45][CH2:44][CH2:43]1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 68511540tert-butyl 4-(1-(4-methoxybenzyl)-4-(2-fluoro-4-(1-(4-fluorophenyl)-6-oxo-1,6-dihydropyridazine-5-carboxamido)phenoxy)-1H-pyrazolo[3,4-b]pyridin-3-yl)-1,4-diazepane-1-carboxylate

Produkt 1

HCID 68515987HCID 68515987, VerbindungAusbeute 58,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A round-bottomed flask was charged with tert-butyl 4-(1-(4-methoxybenzyl)-4-(2-fluoro-4-(1-(4-fluorophenyl)-6-oxo-1,6-dihydropyridazine-5-carboxamido)phenoxy)-1H-pyrazolo[3,4-b]pyridin-3-yl)-1,4-diazepane-1-carboxylate (118.3 mg, 0.1519 mmol), 2,2,2-trifluoroacetic acid (346.4 mg, 3.038 mmol) and CH2Cl2 (10 mL). The reaction mixture was stirred at room temperature for one hour. The solvent was removed and the residue was purified by silica gel chromatography (DCM/7 M NH3 in MeOH from 50/1 to 10/1, v/v) to give product (60.7 mg, 58.88%). LRMS (APCI pos): m/e 679 (M+1).

Aufarbeitung

  1. customThe solvent was removed
  2. customthe residue was purified by silica gel chromatography (DCM/7 M NH3 in MeOH from 50/1 to 10/1

Quellen und Nachweise

ORD-Eintrag
ord-c4d7c53995074ebaa1eb33411fbb290e
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07723330B2

Notizen zur Reaktion

Wird geladen…