HRID476675

反应详情

EQUATION

反应方程式

HRID 476675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the aldehyde from step (d) (14 g) tosic acid (0.2 g) and trimethylorthoformate (6.7 ml) in dry methanol (100 ml) was heated under reflux for 30 mins. A solution of potassium hydroxide in methanol (5 ml) was added to the reaction mixture and the solution evaporated to dryness. The residue was dissolved in ether, washed with water, dried, filtered and evaporated to leave a solid which crystallised from pentane as pale yellow prisms (11.6 g); mp 52.1°-54.0°.

WORKUP

后处理

  1. temperatureunder reflux for 30 mins
  2. customthe solution evaporated to dryness
  3. dissolutionThe residue was dissolved in ether
  4. washwashed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. customto leave a solid which
  9. customcrystallised from pentane as pale yellow prisms (11.6 g)