Phosphorus oxychloride → HCID 57799501, Verbindung

HRID 2100755Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2100755
[CH3:1][N:2]([CH3:25])[C:3]([C:5]1[CH:14]=[C:13]2[C:8]([CH:9]=[C:10]([NH:16][C:17]3[CH:21]=[C:20]([CH3:22])[NH:19][N:18]=3)[N:11]=[C:12]2O)=[CH:7][C:6]=1[O:23][CH3:24])=[O:4].O=P(Cl)(Cl)[Cl:28]>>[CH3:1][N:2]([CH3:25])[C:3]([C:5]1[CH:14]=[C:13]2[C:8]([CH:9]=[C:10]([NH:16][C:17]3[CH:21]=[C:20]([CH3:22])[NH:19][N:18]=3)[N:11]=[C:12]2[Cl:28])=[CH:7][C:6]=1[O:23][CH3:24])=[O:4]

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 178486653HCID 178486653, Verbindung

Produkt 1

HCID 57799501HCID 57799501, VerbindungAusbeute 70 %

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

A mixture of 1-Hydroxy-6-methoxy-3-(5-methyl-1H-pyrazol-3-ylamino)-isoquinoline-7-carboxylic acid dimethylamide (0.1 g, 0.29 mmol) in POCl3 (4 ml) was sealed in microwave process vial (5 ml). The mixture was heated at 130° C. for 30 minutes under microwave irradiation. The mixture was concentrated, and the residue was treated with 1 ml MeOH. After stirred for half an hour at room temperature, the solid was collected and dried to give desired product (0.072 g, 70%). LC-MS: m/e 360 (MH+).

Aufarbeitung

  1. customwas sealed in microwave process vial (5 ml)
  2. concentrationThe mixture was concentrated
  3. additionthe residue was treated with 1 ml MeOH
  4. customthe solid was collected
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-8abf3bc3360d4362a1aaaa7b052899ff
Quelldatensatz
uspto-grants-2009_08
Patentnummer
US07572809B2

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