HRID2061299

反应详情

EQUATION

反应方程式

HRID 2061299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customNext, the ice bath was removed
  2. temperaturea temperature was increased
  3. customa synthesis reaction (see Equation 1 below)
  4. distillationNext, distilled water
  5. additionwas added in a reaction
  6. additionmixed liquid
  7. customthe synthesis reaction
  8. extractionto extract an organic phase
  9. washNext, the organic phase was washed
  10. distillationdistilled water, about 1 N of NaOH aqueous solution
  11. distillationdistilled water in the stated order
  12. customdried
  13. filtrationNext, the organic phase was filtered
  14. concentrationconcentrated