1H-Pyrazol-3-amine, 5-methyl- → HCID 178486653, Verbindung

HRID 2100754Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2100754
[C:1]([CH2:3][C:4]1[C:9]([C:10](O)=[O:11])=[CH:8][C:7]([C:13]([N:15]([CH3:17])[CH3:16])=[O:14])=[C:6]([O:18][CH3:19])[CH:5]=1)#[N:2].[NH2:20][C:21]1[CH:25]=[C:24]([CH3:26])[NH:23][N:22]=1>C(O)(=O)C>[CH3:16][N:15]([CH3:17])[C:13]([C:7]1[CH:8]=[C:9]2[C:4]([CH:3]=[C:1]([NH:20][C:21]3[CH:25]=[C:24]([CH3:26])[NH:23][N:22]=3)[N:2]=[C:10]2[OH:11])=[CH:5][C:6]=1[O:18][CH3:19])=[O:14]

Komponenten

4

Edukt 2

HCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 57799630HCID 57799630, Verbindung

Produkt 1

HCID 178486653HCID 178486653, VerbindungAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

A mixture of 6-Cyanomethyl-4-methoxy-N,N-dimethyl-isophthalamic acid (2.0 g, 7.6 mmol), 3-amino-5-methylpyrazol (1.5 g, 15.44 mmol), acetic acid (10 ml) were sealed in microwave process vial (20 ml). The mixture was heated at 130° C. for 30 minutes under microwave irradiation. After removal of acetic acid, the residue was dissolved in 1.5 ml MeOH, and this solution was added dropwise to 30 ml water. After stirred for 1 hour, the solid was collected and was purified by flash column chromatography to give product (2.2 g, 85%). LC-MS: m/e 342 (MH+).

Aufarbeitung

  1. customwere sealed in microwave process vial (20 ml)
  2. customAfter removal of acetic acid
  3. dissolutionthe residue was dissolved in 1.5 ml MeOH
  4. additionthis solution was added dropwise to 30 ml water
  5. customthe solid was collected
  6. customwas purified by flash column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-83135e71faa54c288857eb4bf2fc2bb0
Quelldatensatz
uspto-grants-2009_08
Patentnummer
US07572809B2

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