HRID1921129

反应详情

EQUATION

反应方程式

HRID 1921129 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 4-(4-cyanophenyl)-6-methyl-2-(methylsulfanyl)-1-[3-(trifluoromethyl)phenyl]-1,4-dihydro-5-pyrimidinecarboxylate (example 7; 100 mg, 0.22 mmol) and sodium methoxide (117.6 mg, 2.18 mmol) are dissolved in 5 ml methanol and stirred at reflux temperature for 3 h. The reaction is quenched with 10 ml of water and the aqueous phase is extracted with 10 ml methylene chloride (2×). After drying with sodium sulfate, the solvent is removed in vacuo and the product is purified by column chromatography (silica gel; eluent: cyclohexane-ethyl acetate, gradient 90:10 to 50:50).

WORKUP

后处理

  1. temperatureat reflux temperature for 3 h
  2. customThe reaction is quenched with 10 ml of water
  3. extractionthe aqueous phase is extracted with 10 ml methylene chloride (2×)
  4. dry with materialAfter drying with sodium sulfate
  5. customthe solvent is removed in vacuo
  6. customthe product is purified by column chromatography (silica gel; eluent: cyclohexane-ethyl acetate, gradient 90:10 to 50:50)