HRID591448
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a mixture of tri-n-butylphosphine (0.338 mL), methyl(7-fluoro-6-hydroxy-4-methyl-1-benzothiophen-3-yl)acetate (131.3 mg), (1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)methanol (93 mg) and THF (4.0 mL) was added ADDP (284 mg) at room temperature. The mixture was stirred overnight at room temperature under nitrogen atmosphere. The mixture was concentrated. 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 compound was crystallized from EtOAc-hexane.
WORKUP
后处理
- concentrationThe mixture was concentrated
- additionTo the residue was added IPE
- filtrationthe precipitate was filtered off
- concentrationThe filtrate was concentrated in vacuo
- customThe residue was purified by silica gel column chromatography (NH, EtOAc/hexane)