反应详情

A mixture of intermediate 2a (0.01 mol) and chloroacetyl chloride (0.0115 mol) in CH2Cl2 (200 ml) was stirred at room temperature. Pyridine (0.02 mol) was added and the mixture was stirred for 2 hours, washed with water, dried, filtered and the solvent was evaporated. The residue was crystallized from MIK/DIPE. The precipitate was filtered off and dried, yielding 6.7 g (87%) [2S-[2α,4α[(R*,R*)]]]-2-[4-[4-[4-[4-[[2-(2,4-difluorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)-1,3-dioxolan-4-yl]methoxy]phenyl]-1-piperazinyl]phenyl]-4,5-dihydro-5-oxo-1H-1,2,4-triazol-1-yl]-1-methylpropyl chloroacetate. (interm.3)

1. stirringthe mixture was stirred for 2 hours
2. washwashed with water
3. customdried
4. filtrationfiltered
5. customthe solvent was evaporated
6. customThe residue was crystallized from MIK/DIPE
7. filtrationThe precipitate was filtered off
8. customdried