HRID1901132
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
A mixture of 2-cyano-4-(3-furyl)-7-iodonaphthalene (1 g), 2-(trimethylsilyl)ethane thiol (390 mg), potassium tert-butoxide (650 mg) and tetrakis (triphenylphosphine)palladium (100 mg) in EtOH (5 mL) was reluxed for 90 min. The solvent was evaporated and the residue partitioned between Et2O and H2O. The organic phase was dried (MgSO4) and concentrated and the residue was dissolved in DMF (24 mL). To this solution was added Bu4NF (7.7 mL of a 1M THF solution). After 30 min., 1N HCl was added followed by H2O. The precipitate that formed was filtered and washed with H2O to provide the title compound as a solid.
WORKUP
后处理
- customThe solvent was evaporated
- customthe residue partitioned between Et2O and H2O
- dry with materialThe organic phase was dried (MgSO4)
- concentrationconcentrated
- dissolutionthe residue was dissolved in DMF (24 mL)
- additionTo this solution was added Bu4NF (7.7 mL of a 1M THF solution)
- waitAfter 30 min.
- addition1N HCl was added
- customThe precipitate that formed
- filtrationwas filtered
- washwashed with H2O