反应详情

2-Chloro-6-fluorobenzyl alcohol (50 g) was stirred in dichloromethane and a solution of sodium hydroxide (32 g) in water was added. After 30 minutes stirring the mixture was cooled to 0° C. when dimethyl sulphate (47 g) and tetrabutyl-ammonium hydrogen-sulphate (1 g) were added dropwise. The mixture was allowed to warm to room temperature and stirred for 3 hours. It was quenched with water and extracted with dichloromethane. The organic extract was washed with water, dried (anhydrous magnesium sulphate) and filtered. The filtrate was evaporated to dryness and the residue distilled under reduced pressure yielding 1-chloro-3-fluoro-2-methoxymethylbenzene (27.3 g) b.p. 82°-95° C./24 mm Hg.

1. additionwere added dropwise
2. stirringstirred for 3 hours
3. customIt was quenched with water
4. extractionextracted with dichloromethane
5. extractionThe organic extract
6. washwas washed with water
7. dry with materialdried (anhydrous magnesium sulphate)
8. filtrationfiltered
9. customThe filtrate was evaporated to dryness
10. distillationthe residue distilled under reduced pressure