HRID623162

反应详情

EQUATION

反应方程式

HRID 623162 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-hydroxy-4-(phenylethynyl)-5-[2-(2,5,5-trimethyl-1,3-dioxan-2-yl)ethyl]-2-cyclohexene-1-one (4 g, 0.011 mole), the title product of Example 1c, pyridinium chloride (2.5 g, 0.022 mole) and absolute methanol (30 mL) were combined and heated to reflux for 4 hr. The reaction mixture was quenched into 50 mL of water, ether was added, the resulting layers separated, the aqueous layer extracted with ether, the ether extracts combined, washed with water, brine, dried over anhydrous Na2SO4, filtered and concentrated in vacuo to give 3.0 g of the title product.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 4 hr
  3. customThe reaction mixture was quenched into 50 mL of water, ether
  4. additionwas added
  5. customthe resulting layers separated
  6. extractionthe aqueous layer extracted with ether
  7. washwashed with water, brine
  8. dry with materialdried over anhydrous Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo