反应详情

To 243 mg (10 mmoles) of magnesium turnings in 10 ml of tetrahydrofuran is added dropwise a solution of 2.69 grams (10 mmoles) of the title product of Example 9 in 5 ml of tetrahydrofuran. After the addition is complete, the mixture is refluxed for one hour. Paraformaldehyde (1.0 g, excess) is then added, and refluxing continued for one hour. The mixture is cooled to room temperature and partitioned between saturated ammonium chloride and diethyl ether. The aqueous layer is further extracted with ether, the combined organic extracts washed with brine, dried over sodium sulfate, filtered, and evaporated. Chromatography of the residue over silica gel using mixtures of ethyl acetate and hexane as eluents gives the title compound.

1. additionAfter the addition
2. temperaturethe mixture is refluxed for one hour
3. temperaturerefluxing
4. custompartitioned between saturated ammonium chloride and diethyl ether
5. extractionThe aqueous layer is further extracted with ether
6. washthe combined organic extracts washed with brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customevaporated