反应详情

Zinc-copper couple (3.21 g, 24.8 mmol) was added to a solution of 2,4-dibromo-6-cyclopropyl-8-(4-(trifluoromethyl)phenylsulfonyl)-8-azabicyclo[3.2.1]oct-6-en-3-one (3.29 g, 6.21 mmol) in a saturated methanolic solution of NH4Cl (24 mL). The reaction mixture was stirred at room temperature for 4 h and was subsequently filtered though Celite. The filtrate was concentrated under vacuum, re-dissolved in CH2Cl2 and washed with saturated aqueous Na2CO3. The organic phase was separated, dried (Na2SO4), filtered, concentrated under vacuum and purified on a silica gel column (eluant hexane/EtOAc, 9/1 to 1/1, v/v) to give compound 116 (1.68 g, 4.52 mmol, 73%). MS (ESI) 372.1 (M+H).

1. filtrationwas subsequently filtered though Celite
2. concentrationThe filtrate was concentrated under vacuum
3. dissolutionre-dissolved in CH2Cl2
4. washwashed with saturated aqueous Na2CO3
5. customThe organic phase was separated
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated under vacuum
9. custompurified on a silica gel column (eluant hexane/EtOAc, 9/1 to 1/1