HRID1614399

反应详情

EQUATION

反应方程式

HRID 1614399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.58 g (4 millimoles) of N-(4-carbethoxyphenyl)-1-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthalenyl)-2-aminoethanol were stirred with 20 ml of 1 N sodium hydrogen phosphite solution and 2 ml (20 millimoles) of formalin solution in 20 ml of dioxane for 1 hour at 60° C. The mixture was then poured onto water and extracted with ether, and the organic phase was washed with 2 N sodium hydroxide solution and water, dried over magnesium sulfate and evaporated down. Recrystallization from methanol gave 1.0 g of the title compound, RF =0.51 (thin layer chromatography, silica gel; 7:1 n-heptane/ethyl acetate).

WORKUP

后处理

  1. additionThe mixture was then poured onto water
  2. extractionextracted with ether
  3. washthe organic phase was washed with 2 N sodium hydroxide solution and water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated down
  6. customRecrystallization from methanol