反应详情

Sodium hydride (11.9 g., 0.050 mole), washed free of mineral oil with hexane, was stirred in 1.8 l. of DMF at ice-water temperature while a solution of 72.3 g (0.40 mole) of 1-phenyl-5-chlorotetrazole and 29.6 g. (0.04 mole) of glycidol in 1.8 l. of DMF was added dropwise during 4 hours. The solution was allowed to stand at 25° overnight (16 hours), diluted with 12 l. of H2O and extracted with ethyl acetate. The extracts were washed with water, dried (Na2SO4), and evaporated to give 75.7 g. of product, m.p. 77°-81°. Recrystallization from MeOH-i-PrOH gave 55.8 g., m.p. 83°-84°.

1. addition(16 hours), diluted with 12 l
2. extractionof H2O and extracted with ethyl acetate
3. washThe extracts were washed with water
4. dry with materialdried (Na2SO4)
5. customevaporated
6. customto give 75.7 g
7. customRecrystallization from MeOH-i-PrOH
8. customgave 55.8 g