Trifluoroacetic acid → 3-Cyano-4-(3-hydroxymethyl-4-phenoxy-phenylamino)-5-methyl-pyrrolo[1,2-b]pyridazine-6-carboxylic acid ethyl ester

HRID 1796632Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1796632
[CH2:1]([O:3][C:4]([C:6]1[C:7]([CH3:39])=[C:8]2[C:13]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([O:21][C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)=[C:17]([CH2:28][O:29]C4CCCCO4)[CH:16]=3)=[C:12]([C:36]#[N:37])[CH:11]=[N:10][N:9]2[CH:38]=1)=[O:5])[CH3:2].C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[C:7]([CH3:39])=[C:8]2[C:13]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([O:21][C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)=[C:17]([CH2:28][OH:29])[CH:16]=3)=[C:12]([C:36]#[N:37])[CH:11]=[N:10][N:9]2[CH:38]=1)=[O:5])[CH3:2]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 69327665HCID 69327665, Verbindung

Produkt 1

HCID 696493093-Cyano-4-(3-hydroxymethyl-4-phenoxy-phenylamino)-5-methyl-pyrrolo[1,2-b]pyridazine-6-carboxylic acid ethyl esterAusbeute 43,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 394 (30 mg, 0.057 mmol) in CH2Cl2 (1 ml) was added TFA (300 μl). The mixture was stirred at rt for 30 min, concentrated and purified by silica gel flash column chromatography to give the title compound (11 mg, 44%) (30% EtOAc—Hexanes). LCMS Found: (M+H)+=443.2

Aufarbeitung

  1. concentrationconcentrated
  2. custompurified by silica gel flash column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-6a7f17bf4de14c848a51bc8bbf22276e
Quelldatensatz
uspto-grants-2006_04
Patentnummer
US07030112B2

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