HRID1072479
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
A mixture of intermediate (9) (0.00183 mole) and NaOH 1N (0.0055 mole) in CH3OH (25 ml) and THF (25 ml) was stirred overnight at RT. The reaction mixture was acidified with 1N HCl (8 ml) and the resulting product was taken up into EtOAc. The organic layer was washed with brine, dried, filtered and the solvent was evaporated. The residue was crystallized from CH3CN. The precipitate was filtered off, washed with DIPE, and dried, yielding 0.8 g (79%) of 2-[1-[2,6-dichloro-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)yl)phenyl]-1-methylethyl]-4-phenyl-5-thiazoleacetic acid (intermediate 10).
WORKUP
后处理
- washThe organic layer was washed with brine
- customdried
- filtrationfiltered
- customthe solvent was evaporated
- customThe residue was crystallized from CH3CN
- filtrationThe precipitate was filtered off
- washwashed with DIPE
- customdried