HRID1176875

反应详情

EQUATION

反应方程式

HRID 1176875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-(4-Bromo-2-methyl-phenylamino)-7-fluoro-3-pent-4-enyl-3H-benzoimidazole-5-carboxylic acid methyl ester 9b is dissolved in 1:1 THF:MeOH (10 mL) and 1 N NaOH solution (2.3 mL) is added. After 5 h, the organic solvents are removed under reduced pressure and the residue diluted with water and 100 mL 1:1 THF:ethyl acetate. The layers are separated and the aqueous layer extracted with ethyl acetate. The combined organic extracts are dried (Na2SO4) and concentrated under reduced pressure to afford 0.39 g (100%) clean desired product as a light yellow solid.

WORKUP

后处理

  1. customthe organic solvents are removed under reduced pressure
  2. additionthe residue diluted with water and 100 mL 1:1 THF
  3. customThe layers are separated
  4. extractionthe aqueous layer extracted with ethyl acetate
  5. dry with materialThe combined organic extracts are dried (Na2SO4)
  6. concentrationconcentrated under reduced pressure