HRID1903423
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
To a solution (15 ml) of 3 g of methyl 21-(2-hydroxy-3,4-dimethoxy-6-methylbenzoyl)heneicosanoate in ethyl acetate are added 0.015 ml of 60% perchloric acid and 600 mg of 5% palladium-on-carbon, and catalytic reduction is carried out at a 70° C. using hydrogen gas at the pressure of 100 kg/cm2. The catalyst is filtered off and the filtrate is washed in sequence with ice water, a saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate. Removal of the solvent by distillation under reduced pressure gives colorless crystals of methyl 22-(2-hydroxy-3,4-dimethoxy-6-methylphenyl)docosanoate. m.p. 71°-72.5° C.
WORKUP
后处理
- customis carried out at a 70° C.
- filtrationThe catalyst is filtered off
- washthe filtrate is washed in sequence with ice water
- dry with materiala saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate
- customRemoval of the solvent
- distillationby distillation under reduced pressure