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HRID 8811作成日:2026年10月26日

1,8-Diazabicyclo(5.4.0)undec-7-ene → 1-[6-(2-Chlorophenyl)-5-(4-chlorophenyl)-3-methylfuro[2,3-b]pyridin-2-yl]-2,2-dimethylpropan-1-one

https://huagongshe.com/reaction/8811

反応式

関与物質

役割名称HCID仕込み量
反応物1,8-Diazabicyclo(5.4.0)undec-7-eneHCID 81184—
反応物1-{[3-Acetyl-6-(2-chlorophenyl)-5-(4-chlorophenyl)pyridin-2-yl]oxy}-3,3-dimethylbutan-2-oneHCID 21984817—
溶媒DimethylformamideHCID 6228—
生成物1-[6-(2-Chlorophenyl)-5-(4-chlorophenyl)-3-methylfuro[2,3-b]pyridin-2-yl]-2,2-dimethylpropan-1-oneHCID 10252566—

反応条件

温度150 °C

反応手順

A mixture of 0.432 g (0.95 mmol) of the product of Step B, 250 A (1.67 mmol) of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) in 2 mL DMF was placed in a 10 mL reaction tube of a CEM Corporation Discover 300 Watt microwave reactor. The reaction vessel was sealed, placed in the microwave reactor and heated at 150° C. for 10 min. After the reaction mixture had cooled to room temperature, it was partitioned between EtOAc and 10% aq. NaHSO4 and extracted. The organic layer was washed with 10% aq. NaHSO4, water, brine, dried (MgSO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–10% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound. HPLC/MS: 438.1 (M+1), 440.1 (M+3); Rt=4.72 min.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07091216B2
出典データセットuspto-grants-2006_08
ORD IDord-3c143f1741694798b05a671e25e7f738
出典メモuspto-grants-2006_08