HRID1832104
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
NBS (0.69 g, 3.85 mmol) was added to a solution of 3-[4-[(4-fluoro-2-{[(methoxycarbonyl)amino]methyl}benzyl)oxy]-6-methyl-2-oxopyridin-1(2H)-yl]-4-methylbenzoic acid (from Step 4) (1.75 g, 3.85 mmol) in DCM (45 mL). After 1.5 h, solvent removed on rotary evaporator. Solid dissolved in EtOAc and hexane added, resulting in a solid precipitate. Solid filtered. Solid subsequently dissolved in DCM and washed with water. Organic layer dried over Na2SO4, filtered, and concentrated. Pale yellow solid dried in vacuo (1.47 g, 72%).
WORKUP
后处理
- customsolvent removed on rotary evaporator
- dissolutionSolid dissolved in EtOAc
- additionhexane added
- customresulting in a solid precipitate
- filtrationSolid filtered
- dissolutionSolid subsequently dissolved in DCM
- washwashed with water
- dry with materialOrganic layer dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customPale yellow solid dried in vacuo (1.47 g, 72%)