HRID390694

反应详情

EQUATION

反应方程式

HRID 390694 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.3 mL (1.3 mmol) of aqueous 1 N lithium hydroxide solution are added to a solution of 423 mg (0.87 mmol) of methyl (Z)-3-[2-butoxy-3′-(3-heptylureido)biphenyl-4-yl]-2-methoxyacrylate in 10 mL of tetrahydrofuran. The reaction mixture is stirred for 24 hours at room temperature. After addition of 20 mL of water and acidification with 1 N hydrochloric acid, the reaction medium is extracted with ethyl acetate. The organic phases are combined, washed with saturated sodium chloride solution and dried over sodium sulfate. The solvents are evaporated off and the residue is then recrystallized from 5 mL of acetonitrile. 348 mg (85%) of (Z)-3-[2-butoxy-3′-(3-heptylureido)biphenyl-4-yl]-2-methoxyacrylic acid are obtained in the form of a white powder. (m.p.=137° C.).

WORKUP

后处理

  1. extractionthe reaction medium is extracted with ethyl acetate
  2. washwashed with saturated sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. customThe solvents are evaporated off
  5. customthe residue is then recrystallized from 5 mL of acetonitrile