反应详情

To a mixture of 1H-tetrazole-5-thiol (27.5 g) and triethylamine (59.9 g) in tetrahydrofuran (550 ml) was added benzhydryl bromide (66.6 g) and then the mixture was refluxed with stirring for 6.5 hours. After the addition of water and ethyl acetate to the reaction mixture, the pH was adjusted to 9.0 with 2N aqueous solution of sodium hydroxide. The aqueous layer was separated and washed with ethyl acetate. After the addition of ethyl acetate to the washed aqueous layer, the mixture was adjusted to pH 2.0 with 10% hydrochloric acid. The ethyl acetate layer was separated, washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate and then evaporated. The residue was pulverized in a mixture of isopropyl ether and n-hexane, collected by filtration, washed with a mixture of isopropyl ether and n-hexane and then dried to give 5-benzhydrylthio-1H-tetrazole (29.62 g), mp 132° to 134° C.

1. temperaturethe mixture was refluxed
2. customThe aqueous layer was separated
3. washwashed with ethyl acetate
4. additionAfter the addition of ethyl acetate to the washed aqueous layer
5. customThe ethyl acetate layer was separated
6. washwashed with a saturated aqueous solution of sodium chloride
7. dry with materialdried over magnesium sulfate
8. customevaporated
9. additionThe residue was pulverized in a mixture of isopropyl ether and n-hexane
10. filtrationcollected by filtration
11. washwashed with a mixture of isopropyl ether and n-hexane
12. customdried