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 methyl 6-((3,5-dichloro-N-(4-fluorobenzyl)-2-hydroxyphenylsulfonamido)methyl)picolinate (0.185 g, 0.37 mmol), 1 N NaOH (2 mL), THF (2 mL) and MeOH (2 mL) was stirred at rt overnight. The reaction mixture was concentrated in vacuo and the residue was diluted with ethyl acetate and 1 N HCl. The organic layer was separated, washed with brine, dried over MgSO4, filtered and the filtrate solution was concentrated to give the desired product (0.18 g, 99%) as a colorless oil. 1H NMR (CDCl3) δ 8.12 (d, J=8.0 Hz, 1H), 7.88 (t, J=8.0 Hz, 1H), 7.58 (d, J=4.0 Hz, 1H), 7.55 (d, J=4.0 Hz, 1H), 7.45 (d, J=8.0 Hz, 1H), 7.06-7.03 (m, 2H), 6.93 (t, J=8.0 Hz, 2H), 4.64 (s, 2H), 4.40 (s, 2H). MS (ESI): 485.0 (M+H)+.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- additionthe residue was diluted with ethyl acetate and 1 N HCl
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationthe filtrate solution was concentrated