反应详情

To a solution of 36.45 g (200 mmol) of 10-undecynoic acid in 200 ml 1 N NaOH at 0° C. was added a solution of alkaline sodium hypobromite dropwise over 30 minutes, maintaining the temperature below 5° C. (the hypobromite solution was prepared by the dropwise addition of 35.16 g (220 mmol) of bromine to 55 ml of 20 N NaOH at 0°-5° C.). The mixture was stirred four hours at 0°-5° C., and was then acidified to PH 1 with 9 M H2SO4. The solution was extracted with three 150 ml portions of ether. The combined extracts were dried (Na2SO4) and evaporated yielding 50.159 (96% crude) of a pale yellow solid. THis was used without further purification.

1. extractionThe solution was extracted with three 150 ml portions of ether
2. dry with materialThe combined extracts were dried (Na2SO4)
3. customevaporated
4. customyielding 50.159 (96% crude) of a pale yellow solid
5. customTHis was used without further purification