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
Under an ice bath, about 200 g of phenol and about 256 g of chloromethyl methyl ether were mixed and stirred in about 2 L of methylene chloride (MC), and about 740 ml of diisopropylethylamine (DIPEA) was gradually dropped. Next, the ice bath was removed and a temperature was increased, and then a synthesis reaction (see Equation 1 below) was performed while stirring for about 12 hours at room temperature. Next, distilled water was added in a reaction mixed liquid to complete the synthesis reaction and to extract an organic phase. Next, the organic phase was washed using about 0.5 N of HCl aqueous solution, distilled water, about 1 N of NaOH aqueous solution, and distilled water in the stated order, and then dried using magnesium sulphate. Next, the organic phase was filtered and concentrated to obtain about 240 g (a yield: about 81.7%) of methoxymethoxybenzene, and a structure of the methoxymethoxybenzene was observed by 1H-NMR (see FIG. 1):
WORKUP
后处理
- customNext, the ice bath was removed
- temperaturea temperature was increased
- customa synthesis reaction (see Equation 1 below)
- distillationNext, distilled water
- additionwas added in a reaction
- additionmixed liquid
- customthe synthesis reaction
- extractionto extract an organic phase
- washNext, the organic phase was washed
- distillationdistilled water, about 1 N of NaOH aqueous solution
- distillationdistilled water in the stated order
- customdried
- filtrationNext, the organic phase was filtered
- concentrationconcentrated