HRID1832104

反应详情

EQUATION

反应方程式

HRID 1832104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customsolvent removed on rotary evaporator
  2. dissolutionSolid dissolved in EtOAc
  3. additionhexane added
  4. customresulting in a solid precipitate
  5. filtrationSolid filtered
  6. dissolutionSolid subsequently dissolved in DCM
  7. washwashed with water
  8. dry with materialOrganic layer dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customPale yellow solid dried in vacuo (1.47 g, 72%)