반응 #321457

반응 방정식

Triethylamine

5-bromo-2-bromomethyl-2,4,6,7-tetramethyl-2,3-dihydrobenzofuran

→

desired compound

수율 92.2%

2-Bromomethyl-2,4,6,7-tetramethyl-2,3-dihydrobenzofuran

수율 92.2%

용매

ethanol

반응 조건

후처리

1. 1
   기타Catalytic hydrogenation decomposition reaction
2. 2
   기타After the completion of the reaction
3. 3
   여과the catalyst was filtered
4. 4
   농축the filtrate was concentrated
5. 5
   workup.DISSOLUTIONThe residue was dissolved in isopropyl ether
6. 6
   세척washed with water
7. 7
   기타dried
8. 8
   workup.DISTILLATIONthe solvent was distilled off
9. 9
   기타The residue was crystallized from methanol

실험 절차

Triethylamine (5.0 ml, 35.6 mmol) was added to a solution of 5-bromo-2-bromomethyl-2,4,6,7-tetramethyl-2,3-dihydrobenzofuran (12.4 g, 35.6 mmol) in ethanol (100 ml). Catalytic hydrogenation decomposition reaction was carried out on 5% palladium carbon under a hydrogen atmosphere. After the completion of the reaction, the catalyst was filtered and the filtrate was concentrated. The residue was dissolved in isopropyl ether, washed with water, dried and the solvent was distilled off. The residue was crystallized from methanol to obtain the desired compound (8.84 g, yield: 92.2%), m.p. 39°-40° C.

출처