반응 #981807

반응 방정식

5-Aminospiro[benzo[b]furan-2(3H),1'-cyclopropane]-3-one

calcium carbonate

bromine

→

5-amino-4-bromospiro[benzo[b]furan-2(3H),1'-cyclopropane]-3-one

용매

carbon tetrachloride

methylene chloride

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate
2. 2
   세척The extract was washed with water
3. 3
   기타dried
4. 4
   기타The solvent was evaporated off
5. 5
   기타the residue was recrystallized from ethanol-water

실험 절차

5-Aminospiro[benzo[b]furan-2(3H),1'-cyclopropane]-3-one (0.747 g.) and calcium carbonate (0.47 g.) were suspended in a mixture of carbon tetrachloride (20 ml.) and methylene chloride (5 ml.). The suspension was cooled to -17° C., then bromine (0.22 ml.) was added thereto dropwise, followed by stirring for 45 minutes. The reaction mixture was poured into ice-water, then extracted with ethyl acetate. The extract was washed with water and dried. The solvent was evaporated off, and the residue was recrystallized from ethanol-water. By the above procedure there was obtained 5-amino-4-bromospiro[benzo[b]furan-2(3H),1'-cyclopropane]-3-one as yellow needles melting at 167°-170° C. Yield 0.6 g.

출처