Ethanol → Methyl 7-(4-butoxyethoxyphenyl)-1-(2-thienylcarbonyl)-2,3-dihydro-1-benzazepine-4-carboxylate

温度

100 °C

In toluene (10 ml), ethanol (1.0 ml) and water (1.0 ml) were suspended methyl 7-bromo-1-(2-thienylcarbonyl)-2,3-dihydro-1-benzazepine-4-carboxylate (210 mg), 4-butoxyethoxyphenyl borate (166 mg) and potassium carbonate (192 mg), and the mixture was stirred for 30 minutes under argon atmosphere. Then, to the suspension was added tetrakistriphenylphosphinepalladium (43 mg), and the mixture was heated at 100° C. for 5 hours under argon atmosphere. After allowing to cool, to the mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried with magnesium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1) to give methyl 7-(4-butoxyethoxyphenyl)-1-(2-thienylcarbonyl)-2,3-dihydro-1-benzazepine-4-carboxylate (201 mg) as colorless oil.

1. temperatureto cool, to the mixture
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with saturated brine
4. dry with materialdried with magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe resulting residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:1)

ORDレコード

ord-426c8912e92042999c94eea477a2a0d0

出典データセット

uspto-grants-2005_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06936602B1