HRID708304

反应详情

EQUATION

反应方程式

HRID 708304 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A tetrahydrofuran solution (30 mL) of the intermediate compound was prepared by the same method described in Example 6 except that 2-methoxymethoxybenzaldehyde (1.2 g) synthesized in the above-described Synthesis Example 2 was used instead of 2,6-dimethylbenzaldehyde (0.65 g). A 6 N hydrochloric acid solution (1 mL) was added to the tetrahydrofuran solution, and the mixture was stirred at 25° C. for 12 hours. After confirmation of the degree of reaction progress by TLC, the reaction was quenched with an aqueous solution of sodium hydrogen carbonate, and the organic phase was extracted with ethyl acetate. The resulting organic phase was dried over anhydrous magnesium sulfate, concentrated, and recrystallized to obtain 1.9 g (yield: 84%) of [4-(2,2-diphenylvinyl)phenyl]-(2-hydroxyphenyl)methanone (10) as yellow crystals. The structure of Product 10 was confirmed by 1H-NMR. Table 1 shows optical characteristics and practical utility of Product 10.

WORKUP

后处理

  1. customsynthesized in the above-described Synthesis Example 2
  2. customAfter confirmation of the degree of reaction progress by TLC
  3. customthe reaction was quenched with an aqueous solution of sodium hydrogen carbonate
  4. extractionthe organic phase was extracted with ethyl acetate
  5. dry with materialThe resulting organic phase was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customrecrystallized