Реакция #67491

Уравнение реакции

KOH

Anisaldehyde

trimethylorthoformate

HCl

→

title compound

Выход 95.2%

1-(dimethoxymethyl)-4-methoxybenzene

Выход 95.2%

Растворители

MeOH

Условия реакции

Обработка

1. 1
   Температураwas warmed to 20-25° C.
2. 2
   workup.STIRRINGfurther stirred for 10 minutes
3. 3
   ЭкстракцияThe reaction mixture was extracted with hexane (2×200 ml)
4. 4
   Промывкаthe combined organic layer was washed with DM water (200 ml)
5. 5
   КонцентрированиеThe organic layer was concentrated below 40° C.

Методика

Anisaldehyde (40 g) and trimethylorthoformate (48.25 ml) were added to MeOH (60 ml) at 20-25° C. and the mixture was cooled to 10-15° C. Conc. HCl (0.26 ml) was then added to the mixture at 10-15° C. and was warmed to 20-25° C. followed by stirring at the same temperature for 16-18 hours. 5% aqueous KOH (40 ml) was added to the reaction mixture at 20-25° C. in 10 min and further stirred for 10 minutes. The reaction mixture was extracted with hexane (2×200 ml) and the combined organic layer was washed with DM water (200 ml). The organic layer was concentrated below 40° C. to obtain title compound (51.0 g, 95.2%).

Источник