反应详情

0.73 g of magnesium turnings are covered with 90 ml of dry diethylether. To that mixture is then added 6 g of 2-bromoindane in 20 ml of dry diethylether at such a rate that a gentle boiling is maintained. When the magnesium turnings have reacted the solution containing the Grignard reagent is cooled to room temperature. The reaction mixture is then added dropwise, over a period of 3 hours, to a cooled (0°-5° C. solution of diethoxyacetic acid piperidinyl amide (6.4 g) in 20 ml of dry diethylether. After the addition is complete, the reaction mixture is stirred for two hours at about 5° C. The mixture is then poured into a cold 2% sulfuric acid solution (50 ml). The solution is extracted with ether and the combined ether extracts are washed with water and evaporated to dryness to give a residue of crude product, which is used without purification in step (b).

1. temperatureis maintained
2. additionThe reaction mixture is then added dropwise, over a period of 3 hours
3. additionAfter the addition
4. extractionThe solution is extracted with ether
5. washthe combined ether extracts are washed with water
6. customevaporated to dryness
7. customto give a residue of crude product, which
8. customis used without purification in step (b)