Phosphorus oxychloride → (1-Chloro-7-fluoro-6-methoxy-isoquinolin-3-yl)-(5-methyl-1H-pyrazol-3-yl)-amine

HRID 2100728

Reaktionsgleichung

Reaktionsgleichung von HRID 2100728
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([NH:13][C:14]3[CH:18]=[C:17]([CH3:19])[NH:16][N:15]=3)[N:8]=[C:9]2O)=[CH:4][C:3]=1[O:20][CH3:21].O=P(Cl)(Cl)[Cl:24]>>[Cl:24][C:9]1[C:10]2[C:5](=[CH:4][C:3]([O:20][CH3:21])=[C:2]([F:1])[CH:11]=2)[CH:6]=[C:7]([NH:13][C:14]2[CH:18]=[C:17]([CH3:19])[NH:16][N:15]=2)[N:8]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 178486654HCID 178486654, Verbindung

Produkt 1

HCID 57799484(1-Chloro-7-fluoro-6-methoxy-isoquinolin-3-yl)-(5-methyl-1H-pyrazol-3-yl)-amineAusbeute 64 %

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

7-Fluoro-6-methoxy-3-(5-methyl-1H-pyrazol-3-ylamino)-isoquinolin-1-ol (1.9 g), POCl3 (15 ml), were sealed in a process vial (20 ml). The mixture was heated at 150° C. for 30 minutes under microwave irradiation. The mixture was concentrated, and the residue was treated with 5 ml MeOH. The mixture was stirred for 2 hours at room temperature, and the solid was collected and dried to give desired product (1.3 g, 64% yield). LC-MS: m/e 307 (MH+)

Aufarbeitung

  1. concentrationThe mixture was concentrated
  2. additionthe residue was treated with 5 ml MeOH
  3. customthe solid was collected
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-edb730d56bfe42ceaec6cbe1d768f33c
Quelldatensatz
uspto-grants-2009_08
Patentnummer
US07572809B2

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