反应详情

To a mixture of tri-n-butylphosphine (0.193 mL), methyl(4,7-dichloro-6-hydroxy-1-benzothiophen-3-yl)acetate (150 mg), (1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)methanol (102 mg) and THF (5.0 mL) was added ADDP (195 mg) at room temperature. The mixture was stirred at room temperature under nitrogen atmosphere overnight. The mixture was concentrated in vacuo. To the residue was added IPE and the precipitate was filtered off. The filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (NH, EtOAc/hexane) to give the title compound (205.9 mg). The solid was crystallized from EtOAc-hexane to give the title compound.

1. concentrationThe mixture was concentrated in vacuo
2. additionTo the residue was added IPE
3. filtrationthe precipitate was filtered off
4. concentrationThe filtrate was concentrated in vacuo
5. customThe residue was purified by silica gel column chromatography (NH, EtOAc/hexane)