Tetrahydrofuran → HCID 178463061, Verbindung

Temperatur

65 °C

A small screw cap test tube was charged with 2-Ethyl-5-methyl-2H-pyrazole-3-carboxylic acid [4-(3-hydroxymethylene-2-oxo-2,3-dihydro-1H-indol-5-ylmethyl)-phenyl]-amide (prepared below, 70 mg, 0.175 mmol) and THF (1 mL). To the resulting solution was added 4-(4-Methyl-piperazin-1-yl)-phenylamine (66.8 mg, 0.349 mmol), and the mixture was stirred for 24 h at 65° C. Subsequently, the reaction mixture was cooled to room temperature and then diluted with EtOAc (2 mL). The solution was washed with water (2 mL) and the water layer was re-washed with additional EtOAc (2 mL). The combined organic layers were then concentrated in vacuo affording the crude product. The crude product was further purified by silica gel column chromatography with 5% methanol in chloroform as eluant to give the desired product as a solid in 55% yield (55 mg, 0.96 mmol).

1. customA small screw cap test tube
2. temperatureSubsequently, the reaction mixture was cooled to room temperature
3. washThe solution was washed with water (2 mL)
4. washthe water layer was re-washed with additional EtOAc (2 mL)
5. concentrationThe combined organic layers were then concentrated in vacuo
6. customaffording the crude product
7. customThe crude product was further purified by silica gel column chromatography with 5% methanol in chloroform as eluant

ORD-Eintrag

ord-099d4d3b51ce4054b735b54975d1806d

Quelldatensatz

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07692005B2