HRID1289390
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
First, 4.9 g of 11-[2,3-difluorobiphenyl-4'-yl]oxyundecyl 2,2-bis(6-benzyloxyhexyl)acetate, 1.5 g of 10% Pd-C, and 100 ml of tetrahydrofuran were placed in a 300 ml autoclave. The mixture was stirred at room temperature for 2 days under a hydrogen pressure of 10 kg/cm2. The catalyst was filtered away and a filtrate was concentrated. Thereafter, the residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=7/3) to obtain 3.7 g of 11-[2,3-difluorobiphenyl-4'-yl]oxyundecyl 2,2-bis(6-hydroxyhexyl)acetate (Y: 97.5%). The compound thus obtained had a purity of 98% by HPLC.
WORKUP
后处理
- filtrationThe catalyst was filtered away
- concentrationa filtrate was concentrated
- customThereafter, the residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=7/3)