HRID2166243

反应详情

EQUATION

反应方程式

HRID 2166243 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2,3,4,5-tetramethoxy-6-methylbenzaldehyde (1.56 g, 6.5 mmol) and acetone (1.13 g, 19.5 mmol) in methanol (15 ml) was added 28% methanolic sodium methoxide (1.88 g). The mixture was refluxed for 1.5 hours. After completion of the reaction, the mixture was concentrated under reduced pressure. The residue was chromatographed ona silica gel column elution being carried out with isopropyl ether. The fractions containing the desired compound were concentrated to give 1,2,3,4-tetramethoxy-5-methyl-6-(3-oxo-1-butenyl)benzene (Compound 21, 1.09 g, 60% Oily substance) δ 2.28 (3H), 2.36 (3H), 3.77 (3H), 3.79 (3H), 3.89 (3H), 3.95 (3H), 6.70 (1H), 7.57 (1H),

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 1.5 hours
  2. customAfter completion of the reaction
  3. concentrationthe mixture was concentrated under reduced pressure
  4. customThe residue was chromatographed ona
  5. washsilica gel column elution
  6. additionThe fractions containing the desired compound
  7. concentrationwere concentrated