HRID2211375

反应详情

EQUATION

反应方程式

HRID 2211375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe mixture was filtered
  2. customthe filtrate evaporated in vacuo
  3. customThe residue was chromatographed on silica gel eluting with dichloromethane/methanol providing 750 mg (84%) of the desired title product
  4. customCrystallization from diethyl ether/hexanes
  5. customgave material with a melting point of 135°-137° C.
  6. customwhen crystallized from toluene