反应详情

A mixture of 2,2-dimethyl-7-hydroxy-4-phenylchroman (3.72 g), sodium hydride (0.53 g, 60% dispersion in oil) and 2-dimethylaminoethyl chloride (1.58 g) in toluene (59 ml) was stirred and boiled under reflux for 6 hours. Water was added to the cooled mixture and the organic layer was separated and extracted with 5 N hydrochloric acid (3×30 ml). The combined acid extract was basified, extracted with ether and the ether extract dried (magnesium sulphate). Removal of the solvent gave 2,2-dimethyl-7-dimethylaminoethoxy-4-phenylchroman which was isolated as its hydrochloride salt, m.p. 165°-167° C.

1. temperatureunder reflux for 6 hours
2. customthe organic layer was separated
3. extractionextracted with 5 N hydrochloric acid (3×30 ml)
4. extractionThe combined acid extract
5. extractionextracted with ether
6. extractionthe ether extract
7. dry with materialdried (magnesium sulphate)
8. customRemoval of the solvent