HRID348507

反应详情

EQUATION

反应方程式

HRID 348507 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A reaction flask was charged with 300 g (1.4 mole) 1,1,2,3,3-pentamethyl-hexahydro-4-indanol, 258 g (2.5 mole) diethoxymethane, 0.25 liter toluene, and 5 g boron trifluoride etherate complex. The reaction mass was heated to 100° C. and methanol and lite organics were collected in a Dean Stark trap (190 g recovered). After aging the reaction for 2 hrs the reaction was cooled to 25° C. and acid catalyst was quenched with 100 g of 10% aqueous sodium carbonate. The mass was transferred to a separatory funnel and water washed. The organic layer was separated and purified by fractional distillation. The procedure afforded a 68% yield (256 g) of 1,1,2,3,3-pentamethyl-octahydro-4-(ethoxymethoxy)-1H-indene.

WORKUP

后处理

  1. custommethanol and lite organics were collected in a Dean Stark trap (190 g recovered)
  2. customthe reaction for 2 hrs the reaction
  3. temperaturewas cooled to 25° C.
  4. customacid catalyst was quenched with 100 g of 10% aqueous sodium carbonate
  5. customThe mass was transferred to a separatory funnel
  6. washwater washed
  7. customThe organic layer was separated
  8. distillationpurified by fractional distillation