8-丙-2-烯氧基-1,4-二氧杂螺[4.5]癸烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 19.8 g of compound (11) (0.1 mmole) were stirred for 2 hours at room temperature with 120 ml ether and 40 ml of 6N hydrochloric acid. The mixture was then neutralised with sodium hydrogen carbonate, extracted three times with ether, and the ether solution was dried over sodium sulphate. After removing the solvent by distillation, 15.2 g of crude product were obtained; the product was purified with 3:1 diisopropyl ether/n-hexane via a silica gel column. extracted three times with ether the ether solution was dried over sodium sulphate After removing the solvent by distillation

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 23.7 g (150 mmole) 1,4-dioxa-spiro[4.5]decan-8-ol were dissolved in 120 ml absolute dimethylformamide under a nitrogen atmosphere. After adding 7.9 g of 50% sodium hydride in mineral oil (165 mmole), the mixture was stirred for 1 hour at 20° C. After adding 14.3 ml allyl bromide (165 mmole), the mixture was heated to 70° C. and stirred for 1 hour. Thereafter it was treated with 160 ml water and was extracted at 10° C.-15° C., three times with ether, once with water and once with saturated sodium chloride solution. After removing the solvent by distillation, 24 g of crude product (81% theoretical) were obtained. the mixture was heated to 70° C. stirred for 1 hour was extracted at 10° C.-15° C. After removing the solvent by distillation

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 23.7 g (150 mmole) 1,4-dioxa-spiro[4.5]decan-8-ol were dissolved in 120 ml absolute dimethylformamide under a nitrogen atmosphere. After adding 7.9 g of 50% sodium hydride in mineral oil (165 mmole), the mixture was stirred for 1 hour at 20° C. After adding 14.3 ml allyl bromide (165 mmole), the mixture was heated to 70° C. and stirred for 1 hour. Thereafter it was treated with 160 ml water and was extracted at 10° C.-15° C., three times with ether, once with water and once with saturated sodium chloride solution. After removing the solvent by distillation, 24 g of crude product (81% theoretical) were obtained. the mixture was heated to 70° C. stirred for 1 hour was extracted at 10° C.-15° C. After removing the solvent by distillation