反应详情

Into a suspension of 1.5 g of 66% sodium hydride-paraffin in 20 cc of dimethylformamide was added a solution of 4.5 g of α-phenyl-α-hydroxyphenylacetic acid in 10 cc of dimethylformamide under cooling, and the mixture was stirred for 1 hour. Successively, 5.8 g of butynyl bromide was added thereto and the stirring was continued for 1 hour. The reaction mixture was poured in ice-water, and the resultant was subjected to extraction with ether. The ether extract was washed with an aqueous solution saturated with sodium chloride, and dried over sodium sulfate. Thereafter ether was distilled out and paraffin was removed to obtain 4.0 g of oily 1-butynyl α-phenyl-α-(1-butynyloxy)phenylacetate, nD25 1.5581.

1. temperatureunder cooling
2. waitthe stirring was continued for 1 hour
3. extractionthe resultant was subjected to extraction with ether
4. extractionThe ether extract
5. washwas washed with an aqueous solution saturated with sodium chloride
6. dry with materialdried over sodium sulfate
7. distillationThereafter ether was distilled out and paraffin
8. customwas removed