반응 #417845

반응 방정식

4,4'-difluorobenzophenone

1,5-dimethyltetrazole

n-butyl lithium

→

title compound

수율 79.0%

1,1-Bis(4-fluorophenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol

수율 79.0%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring for 1 hour at -50° C. and 1 hour at -10° C.
2. 2
   기타the reaction was quenched with 1N hydrochloric acid
3. 3
   추출The mixture was extracted with methylene chloride
4. 4
   기타dried
5. 5
   기타evaporated in vacuo
6. 6
   기타The residue was purified by column chromatography on silica gel eluting with 40% (v/v) ethyl acetate in hexane

실험 절차

To a solution of 1,5-dimethyltetrazole (0.98 g, 10.0 mmoles) in tetrahydrofuran (20 mL) at -30° C. was added n-butyl lithium (4.7 mL of 2.14M solution, 10.0 mmoles). After stirring for 0.25 hour, the solution was cooled to -50° C. and 4,4'-difluorobenzophenone (1.74 g, 8.0 mmoles) was added. After stirring for 1 hour at -50° C. and 1 hour at -10° C., the reaction was quenched with 1N hydrochloric acid. The mixture was extracted with methylene chloride, dried and evaporated in vacuo. The residue was purified by column chromatography on silica gel eluting with 40% (v/v) ethyl acetate in hexane to give 2.0 g of the title compound; m.p.=116°-118° C.

출처