반응 #168280

반응 방정식

4,6-dichloro-3-[(trans-4-methylcyclohexyl)methyl]-3H-imidazo[4,5-c]pyridine

Disodium hydrogen phosphate

1,3-dibromo-5,5-dimethylhydantoin

→

2-bromo-4,6-dichloro-3-[(trans-4-methylcyclohexyl)methyl]-3H-imidazo[4,5-c]pyridine

용매

THF

EtOAc

반응 조건

후처리

1. 1
   workup.STIRRINGwith stirring at 35° C
2. 2
   세척washed with aqueous NaHSO3 and brine
3. 3
   건조The organic layer was dried over Na2SO4
4. 4
   여과filtered
5. 5
   농축concentrated
6. 6
   기타Purification of the residue on a silica gel column with 0 to 50% EtOAc/hexanes

실험 절차

4,6-dichloro-3-[(trans-4-methylcyclohexyl)methyl]-3H-imidazo[4,5-c]pyridine (1 g, 3.35 mmol) was dissolved in THF (10 mL). Disodium hydrogen phosphate (1.43 g, 10.1 mmol) was added, and the reaction was warmed to 35° C. with stirring. 1,3-dibromo-5,5-dimethylhydantoin (1.15 g, 4.02 mmol) was added in 1 portion, and the reaction was continued with stirring at 35° C. After 45 minutes, the reaction was diluted with EtOAc (100 mL) and washed with aqueous NaHSO3 and brine. The organic layer was dried over Na2SO4, filtered, and concentrated. Purification of the residue on a silica gel column with 0 to 50% EtOAc/hexanes provided 2-bromo-4,6-dichloro-3-[(trans-4-methylcyclohexyl)methyl]-3H-imidazo[4,5-c]pyridine.

출처