HRID342327

反应详情

EQUATION

反应方程式

HRID 342327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Propyl-1,3-propanediol (138.0 g; 1.17 mol) and 3-fluorobenzaldehyde (138.0 g; 1.11 mol) were dissolved in toluene (1.5 liters), and PTS (7 g) was added. The mixture was refluxed for 3 hours while being dehydrated with a Dean-Stark's device. The resultant reaction mixture was washed sequentially with saturated sodium bicarbonate solution and saturated brine, and then dried over magnesium sulfate. Subsequently, the solvent was evaporated. The residue was recrystallized twice from heptane, to thereby obtain 81.2 g (362 mmol) of 5-propyl-2-(3-fluorophenyl)-1,3-dioxane. The yield of the compound from 3-fluorobenzaldehyde was 32.6%.

WORKUP

后处理

  1. additionPTS (7 g) was added
  2. temperatureThe mixture was refluxed for 3 hours
  3. customThe resultant reaction mixture
  4. washwas washed sequentially with saturated sodium bicarbonate solution and saturated brine
  5. dry with materialdried over magnesium sulfate
  6. customSubsequently, the solvent was evaporated
  7. customThe residue was recrystallized twice from heptane