HRID1460246
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 10.0 g (0.3 mole) α,α-bis(4-fluoropheny)-4-pyridineethanol and 1.2 g of 5% platinum on carbon catalyst in 200 ml of acetic acid was shaken under an atmosphere of hydrogen (49 psi) for 16 hr. The solution was filtered through Celite®, and the solvent was removed in vacuo. The residue was partitioned between methylene chloride and dilute sodium hydroxide. The solvent was removed in vacuo to give an oil. This was dissolved in methanol, an excess of ethereal hydrogen chloride was added and ether was added. A precipitate was collected to give 7.58 g (72%) as a white crystalline solid, mp 171°-173° C.
WORKUP
后处理
- filtrationThe solution was filtered through Celite®
- customthe solvent was removed in vacuo
- customThe residue was partitioned between methylene chloride and dilute sodium hydroxide
- customThe solvent was removed in vacuo
- customto give an oil
- customA precipitate was collected
- customto give 7.58 g (72%) as a white crystalline solid, mp 171°-173° C.