反应详情

To a solution of 660 mg. of 4-[4(2,3-epoxypropoxy)phenyl]-1,2,3-thiadiazole in 29.7 ml. of t-butylamine is added 3.3 ml. of t-butanol and the reaction mixture is stirred at room temperature for 24 hours. It is then evaporated to dryness under vacuo and the residue taken up in methylene chloride. The resulting solution is extracted with dilute hydrochloric acid and the aqueous phase made alkaline with sodium carbonate. It is then extracted with ethyl acetate and the organic extracts washed to neutrality, dried over sodium sulfate and evaporated to dryness. The solid residue is purified by two recrystallizations from methylene chloridehexane (after decolorization with charcoal) and then by three crystallizations from benzene, thus obtaining the pure 4-[4(3-t-butylamino-2-hydroxypropoxy)phenyl]-1,2,3-thiadiazole, m.p. 124°-125° C; λmax 256, 304 nm, (ε 20,000;2,000) ir 3340, 1615, 1580, 1535, 835 cm-1.

1. customIt is then evaporated to dryness under vacuo
2. extractionThe resulting solution is extracted with dilute hydrochloric acid
3. extractionIt is then extracted with ethyl acetate
4. washthe organic extracts washed to neutrality
5. dry with materialdried over sodium sulfate
6. customevaporated to dryness
7. customThe solid residue is purified by two recrystallizations from methylene chloridehexane (after decolorization with charcoal)
8. customby three crystallizations from benzene