反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Sodium hydroborate (0.001 mol) was added portionwise at room temperature to a mixture of intermediate 8 (0.001 mol) in methanol (5 ml). The mixture was stirred at room temperature for 2 hours and poured out into ice water. DCM was added. The organic layer was washed with water, separated, dried (MgSO4), filtered and the solvent was evaporated. The residue was crystallized from 2-propanone. The precipitate was filtered off and dried in a vacuo. The residue (0.35 g, 70%) was crystallized from ethanol. The precipitate was filtered off and dried in a vacuo, yielding 0.105 g (21%) of 5-(3-chlorophenyl)-α-(4-fluorophenyl)-4,5-dihydro-α-(1-methyl-1H-imidazol-5-yl)- tetrazolo[1,5-α]quinazoline-7-methanol (intermediate 9), mp. 230° C.
WORKUP
后处理
- washThe organic layer was washed with water
- customseparated
- dry with materialdried (MgSO4)
- filtrationfiltered
- customthe solvent was evaporated
- customThe residue was crystallized from 2-propanone
- filtrationThe precipitate was filtered off
- customdried in a vacuo
- customThe residue (0.35 g, 70%) was crystallized from ethanol
- filtrationThe precipitate was filtered off
- customdried in a vacuo