HRID1787398

反应详情

EQUATION

反应方程式

HRID 1787398 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Second Step: 267.3 g of the compound (11), 5.0 g of Pd/C, 500 mL of isopropyl alcohol (IPA) and 500 mL of toluene were added to a reactor, and stirred under hydrogen atmosphere for 24 hours. After confirming that the reaction had been completed by GC analysis, the Pd/C was filtered off, and the solvent was removed by distillation under reduced pressure to obtain a residue. The resulting residue was purified by silica gel column chromatography using heptane as eluent, and the solvent was distilled off under reduced pressure to obtain 255.2 g of (1,4-dioxaspiro[4,5]dec-8-yl)acetic acid ethyl ester (12) as a colorless liquid.

WORKUP

后处理

  1. filtrationthe Pd/C was filtered off
  2. customthe solvent was removed by distillation under reduced pressure
  3. customto obtain a residue
  4. customThe resulting residue was purified by silica gel column chromatography
  5. distillationthe solvent was distilled off under reduced pressure