HRID247357

反应详情

EQUATION

反应方程式

HRID 247357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 730 g (5 mol) of 2,5-dimethylhexane-2,5-diol, 3 g of p-toluenesulfonic acid, 430 g (5 mol) of pivalaldehyde and 1 l of toluene was refluxed for 4 hours (h) during which the water of reaction produced (90 ml) was removed. The reaction mixture was then cooled down to room temperature (RT) and stirred up with 10 ml of 25% strength aqueous sodium hydroxide solution, the phases were separated, the organic phase was washed with a little water until neutral, and the toluene was then removed at 50°-60° C. The residue obtained was fractionated under reduced pressure affording 909 g (4.25 mol) of 2-tert.-butyl-4,4,7,7,-tetramethyl-1,3-dioxacycloheptane (boiling point 54° C./0.2 mbar). This corresponds to a yield of 85% of theory.

WORKUP

后处理

  1. temperaturewas refluxed for 4 hours (h) during which
  2. customproduced (90 ml)
  3. customwas removed
  4. customthe phases were separated
  5. washthe organic phase was washed with a little water until neutral, and the toluene
  6. customwas then removed at 50°-60° C
  7. customThe residue obtained