HRID2211375
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 1.1 g of 2-methyl-2-(1H-tetrazol-5-yl)-7-(2-ethyl-4-(4-fluorophenyl)-5-benzyloxyphenoxy)heptane, 1 g of 10% palladium on carbon, and 200 mL of ethanol was hydrogenated on a Parr™ apparatus at 35-40 psi for 2 hours. The mixture was filtered and the filtrate evaporated in vacuo. The residue was chromatographed on silica gel eluting with dichloromethane/methanol providing 750 mg (84%) of the desired title product. MS, NMR. Crystallization from diethyl ether/hexanes gave material with a melting point of 135°-137° C.; when crystallized from toluene, the melting point was 142°-143° C.
WORKUP
后处理
- filtrationThe mixture was filtered
- customthe filtrate evaporated in vacuo
- customThe residue was chromatographed on silica gel eluting with dichloromethane/methanol providing 750 mg (84%) of the desired title product
- customCrystallization from diethyl ether/hexanes
- customgave material with a melting point of 135°-137° C.
- customwhen crystallized from toluene